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Advances in Food Analysis

A topical collection in Molecules (ISSN 1420-3049). This collection belongs to the section "Analytical Chemistry".

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Editors

Department of Chemistry, Sapienza University, 00185 Rome, Italy
Interests: liquid chromatography; mass spectrometry; development of original extraction procedures (e.g., SPE prototypes, evaluation of last-generation materials as sorbents for SPE and liquid ionic/deep eutectic solvents for DLLME); development and validation of LC methods; LC-DAD-MS/MS profiling of organic micronutrients in foods and biological fluids
Special Issues, Collections and Topics in MDPI journals
Department of Science and Technology for Humans and the Environment, Campus Bio-Medico University of Rome, Via Alvaro del Portillo 21, 00128 Rome, Italy
Interests: chromatography; mass spectrometry; HPLC; sample preparation; analytical chemistry instrumentation; liquid chromatography; analytical method development; chromatographic method development; ESI
Special Issues, Collections and Topics in MDPI journals

Topical Collection Information

Dear Colleagues,

Nowadays, the growing awareness of the close relation among diet, health and social development is stimulating demands for high levels of quality and safety in agro-food production, as well as new studies to fill gaps in the actual body of knowledge about food composition. For these reasons, modern research in food science and human nutrition is moving from classical methodologies to advanced instrumental platforms for comprehensive characterization. Non-destructive spectroscopic and imaging technologies are also proposed for food process monitoring and quality control in real-time.

This Special Issue is intended to highlight the most recent advancements and trends within the framework of food analysis. Research papers and reviews illustrating the most interesting developments related to sample preparation, separation science, spectroscopic techniques, sensors and biosensors, as well as investigations dealing with characterization of macronutrients, micronutrients and other biomolecules of interest are welcome.

We warmly invite our colleagues to submit their original contributions to this Special Issue in order to provide updates regarding alternative food sources (e.g., algae), functional foods, chiral or achiral bioactive compounds, effects of processing, contaminants, and every topic related to food science that is appealing to readers.

We would be delighted if you could respond to confirm your contribution and the proposed title by 30 November, 2018.

Prof. Dr. Alessandra Gentili
Prof. Dr. Chiara Fanali
Guest Editors

Manuscript Submission Information

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Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Molecules is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2700 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • sample preparation
  • separation techniques
  • sensor analysis
  • spectroscopic techniques
  • food composition
  • food contaminants
  • natural products
  • characterization of alternative food sources
  • characterization of medicinal herbs

Published Papers (48 papers)

2024

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19 pages, 1838 KiB  
Article
Artificial Intelligence Sensing: Effective Flavor Blueprinting of Tea Infusions for a Quality Control Perspective
by Andrea Caratti, Angelica Fina, Fulvia Trapani, Carlo Bicchi, Erica Liberto, Chiara Cordero and Federico Magagna
Molecules 2024, 29(3), 565; https://doi.org/10.3390/molecules29030565 - 23 Jan 2024
Viewed by 527
Abstract
Tea infusions are the most consumed beverages in the world after water; their pleasant yet peculiar flavor profile drives consumer choice and acceptance and becomes a fundamental benchmark for the industry. Any qualification method capable of objectifying the product’s sensory features effectively supports [...] Read more.
Tea infusions are the most consumed beverages in the world after water; their pleasant yet peculiar flavor profile drives consumer choice and acceptance and becomes a fundamental benchmark for the industry. Any qualification method capable of objectifying the product’s sensory features effectively supports industrial quality control laboratories in guaranteeing high sample throughputs even without human panel intervention. The current study presents an integrated analytical strategy acting as an Artificial Intelligence decision tool for black tea infusion aroma and taste blueprinting. Key markers validated by sensomics are accurately quantified in a wide dynamic range of concentrations. Thirteen key aromas are quantitatively assessed by standard addition with in-solution solid-phase microextraction sampling followed by GC-MS. On the other hand, nineteen key taste and quality markers are quantified by external standard calibration and LC-UV/DAD. The large dynamic range of concentration for sensory markers is reflected in the selection of seven high-quality teas from different geographical areas (Ceylon, Darjeeling Testa Valley and Castleton, Assam, Yunnan, Azores, and Kenya). The strategy as a sensomics-based expert system predicts teas’ sensory features and acts as an AI smelling and taste machine suitable for quality controls. Full article
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2023

Jump to: 2024, 2022, 2021, 2020, 2019, 2018

17 pages, 2150 KiB  
Article
Comparative Performance of Rapid Diagnostics for the Detection of T-2 and HT-2 Toxins in Oats
by Julie Meneely, Brett Greer, Oluwatobi Kolawole, Qiqi He and Christopher Elliott
Molecules 2023, 28(18), 6657; https://doi.org/10.3390/molecules28186657 - 16 Sep 2023
Viewed by 665
Abstract
The contamination of oat crops by trichothecene mycotoxins, T-2 and HT-2 is an ongoing threat to our food safety. Within the industry, there are increasing concerns about the continued and growing presence of these mycotoxins occurring in oat crops due to climate change, [...] Read more.
The contamination of oat crops by trichothecene mycotoxins, T-2 and HT-2 is an ongoing threat to our food safety. Within the industry, there are increasing concerns about the continued and growing presence of these mycotoxins occurring in oat crops due to climate change, farming practices and the handling of crops post-harvest. To safeguard human health, monitoring these mycotoxins in foodstuffs is paramount to ensure human exposure is limited. To achieve this, effective testing regimes must be established within the industry, consisting not only of rapid, reliable, and accurate analytical methods but also efficient sampling strategies. Four commercial rapid diagnostic kits were assessed against liquid chromatography coupled to mass spectrometry and included three lateral flow devices and one enzyme-linked immunosorbent assay. One-way ANOVA showed a p-value of 0.45 indicating no significant difference between the methods assessed. Qualitative analysis revealed test kits 1, 2, 3, and 4 showed false negative/false positive rates of 1.1/2.2, 7.6/0, 2.2/0, and 6.5/0 percent, respectively. Test Kit 1, the Neogen Reveal® Q+ MAX for T-2/HT-2 Kit provided the most reliable, accurate and cost-effective results. Furthermore, its ease of use and no requirement for technical skill makes it applicable for on-site testing. Full article
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14 pages, 3479 KiB  
Article
Rapid Limit Test of Eight Quinolone Residues in Food Based on TLC-SERS, a New Limit Test Method
by Honglian Zhang, Min Zhang, Li Li, Wei Dong, Qiyong Ren, Feng Xu, Yuanrui Wang, Tao Xu and Jicheng Liu
Molecules 2023, 28(18), 6473; https://doi.org/10.3390/molecules28186473 - 06 Sep 2023
Viewed by 722
Abstract
Residual quinolones in food that exceed their maximum residue limit (MRL) are harmful to human health. However, the existing methods used for testing these residues have limitations; so, we developed a new limit test method called TLC-SERS to rapidly determine the levels of [...] Read more.
Residual quinolones in food that exceed their maximum residue limit (MRL) are harmful to human health. However, the existing methods used for testing these residues have limitations; so, we developed a new limit test method called TLC-SERS to rapidly determine the levels of residues of the following: enrofloxacin (A), ciprofloxacin (B), ofloxacin (C), fleroxacin (D), sparfloxacin (E), enoxacin (F), gatifloxacin (G), and nadifloxacin (H). The residues ware preliminarily separated via TLC. The tested compounds’ position on a thin-layer plate were labeled using their relative Rf under 254 nm ultraviolet light, and an appropriate amount of nanometer silver solution was added to the position. The silver on the plate was irradiated with a 532 nm laser to obtain the SERSs of the compounds. The results show significant differences in the SERS of the eight quinolones: the LODs of H, A, D, E, C, G, F, and B were 9.0, 12.6, 8.9, 19.0, 8.0, 8.7, 19.0, and 12.6 ng/mL, respectively; and the RSD was ≤4.9% for the SERS of each quinolone. The limit test results of 20 samples are consistent with those obtained via UPLC–MS/MS. The results indicate that TLC-SERS is a specific, sensitive, stable, and accurate method, providing a new reference for the rapid limit test of harmful residues in foods. Full article
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2022

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11 pages, 7664 KiB  
Article
Chemometric Classification of Colombian Cacao Crops: Effects of Different Genotypes and Origins in Different Years of Harvest on Levels of Flavonoid and Methylxanthine Metabolites in Raw Cacao Beans
by Catalina Agudelo, Susana Acevedo, Luis Carrillo-Hormaza, Elkin Galeano and Edison Osorio
Molecules 2022, 27(7), 2068; https://doi.org/10.3390/molecules27072068 - 23 Mar 2022
Cited by 2 | Viewed by 2114
Abstract
The aim of this study was to evaluate the levels of chemical markers in raw cacao beans in two clones (introduced and regional) in Colombia over several years. Multivariate statistical methods were used to analyze the flavanol monomers (epicatechin and catechin), flavanol oligomers [...] Read more.
The aim of this study was to evaluate the levels of chemical markers in raw cacao beans in two clones (introduced and regional) in Colombia over several years. Multivariate statistical methods were used to analyze the flavanol monomers (epicatechin and catechin), flavanol oligomers (procyanidins) and methylxanthine alkaloids (caffeine and theobromine) of cocoa samples. The results identified genotype as the main factor contributing to cacao chemistry, although significant differences were not observed between universal and regional clones in PCA. The univariate analysis allowed us to establish that EET-96 had the highest contents of both flavanol monomers (13.12 ± 2.30 mg/g) and procyanidins (7.56 ± 4.59 mg/g). In addition, the geographic origin, the harvest conditions of each region and the year of harvest may contribute to major discrepancies between results. Turbo cocoa samples are notable for their higher flavanol monomer content, Chigorodó cocoa samples for the presence of both types of polyphenol (monomer and procyanidin contents) and the Northeast cocoa samples for the higher methylxanthine content. We hope that knowledge of the heterogeneity of the metabolites of interest in each clone will contribute to the generation of added value in the cocoa production chain and its sustainability. Full article
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2021

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18 pages, 3180 KiB  
Review
Mimotopes for Mycotoxins Diagnosis Based on Random Peptides or Recombinant Antibodies from Phage Library
by Wei Sun, Yan Zhang and Zhigang Ju
Molecules 2021, 26(24), 7652; https://doi.org/10.3390/molecules26247652 - 17 Dec 2021
Cited by 6 | Viewed by 2811
Abstract
Mycotoxins, the small size secondary metabolites of fungi, have posed a threat to the safety of medicine, food and public health. Therefore, it is essential to create sensitive and effective determination of mycotoxins. Based on the special affinity between antibody and antigen, immunoassay [...] Read more.
Mycotoxins, the small size secondary metabolites of fungi, have posed a threat to the safety of medicine, food and public health. Therefore, it is essential to create sensitive and effective determination of mycotoxins. Based on the special affinity between antibody and antigen, immunoassay has been proved to be a powerful technology for the detection of small analytes. However, the tedious preparation and instability of conventional antibodies restrict its application on easy and fast mycotoxins detection. By virtue of simplicity, ease of use, and lower cost, phage display library provides novel choices for antibodies or hapten conjugates, and lead random peptide or recombinant antibody to becoming the promising and environmental friendly immune-reagents in the next generation of immunoassays. This review briefly describes the latest developments on mycotoxins detection using M13 phage display, mainly focusing on the recent applications of phage display technology employed in mycotoxins detection, including the introduction of phage and phage display, the types of phage displayed peptide/recombinant antibody library, random peptides/recombinant antibodies-based immunoassays, as well as simultaneous determination of multiple mycotoxins. Full article
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12 pages, 1098 KiB  
Article
Sensory-Based Identification of Aroma-Active Compounds in Hotpot Seasoning before and after Boiling
by Mingguang Yu, Suyan Wan, Huanlu Song, Yu Zhang, Chuanming Wang, Hongqiang Wang and Haowen Wang
Molecules 2021, 26(19), 5727; https://doi.org/10.3390/molecules26195727 - 22 Sep 2021
Cited by 11 | Viewed by 2329
Abstract
Boiling, the most frequent edible way to hotpot seasoning (HS), exerts a significant impact on the aroma of HS. The present study employed, for the first time, a novel switchable system between GC-O-MS and GC×GC-O-MS (SGC/GC×GC-O-MS) to study the aroma compounds of HS [...] Read more.
Boiling, the most frequent edible way to hotpot seasoning (HS), exerts a significant impact on the aroma of HS. The present study employed, for the first time, a novel switchable system between GC-O-MS and GC×GC-O-MS (SGC/GC×GC-O-MS) to study the aroma compounds of HS and hotpot seasoning boiling liquid (HSBL). A total of 79 aroma compounds and 56 aroma-active compounds were identified. The aroma extract dilution analysis (AEDA) was used to analyze the differences between the key aroma-active components in the HS and HSBL. The results showed that 13 aroma-active components were significantly affected by boiling, such as D-limonene, methional, and linalool. Moreover, a total of 22 key aroma-active components were identified through the odor activity values (OAVs) calculation. Of them, (E)-2-octenal (fatty) and linalool showed a significant difference, suggesting them to be the most critical aroma-active compounds in the HSBL, and HS, respectively. Finally, the correlation between key aroma-active compounds and the sensory properties of HS and HSBL was studied. These results demonstrated that the OAVs of key aroma-active compounds could characterize the real information of samples through bidirectional orthogonal partial least squares (O2PLS). The analysis results were consistent with the sensory evaluation results. Full article
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12 pages, 3012 KiB  
Article
Analytical Problems in Separation of Selenomethionine and Its Oxidative Product in HILIC HPLC
by Aleksandra Sentkowska and Krystyna Pyrzynska
Molecules 2021, 26(16), 5073; https://doi.org/10.3390/molecules26165073 - 21 Aug 2021
Cited by 6 | Viewed by 1610
Abstract
Selenomethionine (SeMet) is one of the main selenium forms in foods and supplements. Determining its presence in natural food samples creates difficulties due to possible oxidation processes. The objective of this study was to evaluate the possible degradation of SeMet in water extracts [...] Read more.
Selenomethionine (SeMet) is one of the main selenium forms in foods and supplements. Determining its presence in natural food samples creates difficulties due to possible oxidation processes. The objective of this study was to evaluate the possible degradation of SeMet in water extracts of green teas, one of the most consumed beverages worldwide. Such a medium has not been investigated at this time. The HILIC-HPLC MS/MS method with different stationary phases was used to achieve the satisfactory separation of SeMet and selenomethionine oxide (SeMetO). The addition of dithiothreitol and β-mercaptoethanol, recommended to ensure that SeMet is kept in the reduced form, was also evaluated. The best separation was achieved using the zwitterionic HILIC stationary phase coupled to mass spectrometry and MeOH with water (85/15, v/v) as the eluent. Extraction was done with hot water with the addition of β-mercaptoethanol. The infusions prepared from Lung-Ching teas (from the Zhejiang Province in China) contained the highest concentration of selenium in a typical cup of tea (12.5–17.3 µg L−1). For other tested teas it decreased in the following order: Yunnan > Dilmah > Lipton. For Lung-Ching teas, the sum of concentrations of SeMet and SeMetO corresponded to about 46–63% of the total selenium in their extracts. Full article
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19 pages, 4132 KiB  
Review
Laser-Induced Breakdown Spectroscopy: An Efficient Tool for Food Science and Technology (from the Analysis of Martian Rocks to the Analysis of Olive Oil, Honey, Milk, and Other Natural Earth Products)
by Dimitrios Stefas, Nikolaos Gyftokostas, Eleni Nanou, Panagiotis Kourelias and Stelios Couris
Molecules 2021, 26(16), 4981; https://doi.org/10.3390/molecules26164981 - 17 Aug 2021
Cited by 13 | Viewed by 3264
Abstract
Laser-Induced Breakdown Spectroscopy (LIBS), having reached a level of maturity during the last few years, is generally considered as a very powerful and efficient analytical tool, and it has been proposed for a broad range of applications, extending from space exploration down to [...] Read more.
Laser-Induced Breakdown Spectroscopy (LIBS), having reached a level of maturity during the last few years, is generally considered as a very powerful and efficient analytical tool, and it has been proposed for a broad range of applications, extending from space exploration down to terrestrial applications, from cultural heritage to food science and security. Over the last decade, there has been a rapidly growing sub-field concerning the application of LIBS for food analysis, safety, and security, which along with the implementation of machine learning and chemometric algorithms opens new perspectives and possibilities. The present review intends to provide a short overview of the current state-of-the-art research activities concerning the application of LIBS for the analysis of foodstuffs, with the emphasis given to olive oil, honey, and milk. Full article
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2020

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11 pages, 1233 KiB  
Article
Determination of Triacylglycerols by HTGC-FID as a Sensitive Tool for the Identification of Rapeseed and Olive Oil Adulteration
by Ying Qian, Magdalena Rudzińska, Anna Grygier and Roman Przybylski
Molecules 2020, 25(17), 3881; https://doi.org/10.3390/molecules25173881 - 26 Aug 2020
Cited by 14 | Viewed by 2847
Abstract
Triacylglycerols (TGs) are the most common compounds in food lipids, accounting for 95% of the weight of edible oils. The aim of this study was to scrutinize a procedure for quantitatively assessing possible adulteration of olive and rapeseed oil through GC-FID analysis of [...] Read more.
Triacylglycerols (TGs) are the most common compounds in food lipids, accounting for 95% of the weight of edible oils. The aim of this study was to scrutinize a procedure for quantitatively assessing possible adulteration of olive and rapeseed oil through GC-FID analysis of TGs. The recovery of TG standards ranged from 21% to 148%, and the relative response factor (RRF) ranged from 0.42 to 2.28. The limits of detection were in the range of 0.001 to 0.330 µg/mL, and the limits of quantitation from 0.001 to 1.000 µg/mL. The validated method was used to determine the TGs in olive oil (OO), refined rapeseed oil (RRO), and their blends. Eight TGs were detected in refined rapeseed oil, and 10 in olive oil. The addition of 1% of olive oil to rapeseed oil or vice versa can be detected using this method. Three triacylglycerols were pinpointed as indicators of adulteration of rapeseed oil with olive oil (PPO, PPL, PSO). The method described here can be used for controlling the quality of these oils. Full article
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16 pages, 552 KiB  
Review
Spray Drying for the Encapsulation of Oils—A Review
by Nameer Khairullah Mohammed, Chin Ping Tan, Yazid Abd Manap, Belal J. Muhialdin and Anis Shobirin Meor Hussin
Molecules 2020, 25(17), 3873; https://doi.org/10.3390/molecules25173873 - 26 Aug 2020
Cited by 115 | Viewed by 10018
Abstract
The application of the spray drying technique in the food industry for the production of a broad range of ingredients has become highly desirable compared to other drying techniques. Recently, the spray drying technique has been applied extensively for the production of functional [...] Read more.
The application of the spray drying technique in the food industry for the production of a broad range of ingredients has become highly desirable compared to other drying techniques. Recently, the spray drying technique has been applied extensively for the production of functional foods, pharmaceuticals and nutraceuticals. Encapsulation using spray drying is highly preferred due to economic advantages compared to other encapsulation methods. Encapsulation of oils using the spray drying technique is carried out in order to enhance the handling properties of the products and to improve oxidation stability by protecting the bioactive compounds. Encapsulation of oils involves several parameters—including inlet and outlet temperatures, total solids, and the type of wall materials—that significantly affect the quality of final product. Therefore, this review highlights the application and optimization of the spray drying process for the encapsulation of oils used as food ingredients. Full article
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13 pages, 252 KiB  
Article
Pu-erh Tea Extract Treatment Could Be an Efficient Way to Enhance the Yield and Nutritional Value of Soybean Sprout
by Jeong-Ho Kim, Yong-Han Yoon, Il-Doo Kim, Sanjeev Kumar Dhungana and Dong-Hyun Shin
Molecules 2020, 25(17), 3869; https://doi.org/10.3390/molecules25173869 - 25 Aug 2020
Cited by 4 | Viewed by 2466
Abstract
Soybean sprouts are one of the most inexpensive and nutritious food items that can be easily grown year-round. Several studies have been conducted to increase their yield and nutritional values. This study was carried out to examine the effects of Pu-erh tea extracts [...] Read more.
Soybean sprouts are one of the most inexpensive and nutritious food items that can be easily grown year-round. Several studies have been conducted to increase their yield and nutritional values. This study was carried out to examine the effects of Pu-erh tea extracts on the production and nutrients content of soybean sprouts. Soybean seeds were soaked in 1%, 2%, or 3% (w/v) tea extracts, or tap water, before keeping for sprout cultivation; the sprout samples were named PE-1, PE-2, PE-3, and the control, respectively. The sprout yields were increased by up to 17% in PE-2 and PE-3 than in the control. The vitamin C, total free amino acid, total mineral, total isoflavone, total polyphenol, and flavonoid contents as well as the antioxidant potentials of the tea extract-treated sprouts were higher than those of the control. The results indicated that pre-soaking soybean seeds in 2% Pu-erh tea extracts could offer an easy, inexpensive, and efficient way to improve the yield and nutritional value of soybean sprouts. Full article
30 pages, 3014 KiB  
Article
Study on Effect of Extraction Techniques and Seed Coat on Proteomic Distribution and Cheese Production from Soybean Milk
by Nadia Al-Saedi, Manjree Agarwal, Wujun Ma, Shahidul Islam and Yonglin Ren
Molecules 2020, 25(14), 3237; https://doi.org/10.3390/molecules25143237 - 16 Jul 2020
Cited by 2 | Viewed by 2729
Abstract
Soybean-based food products are a major source of protein. In the present study, proteins in soybean milk from seeds of the cultivar Bunya (Glycine max) were extracted using the cheesecloth and the centrifuge methods. The milk was produced through mechanical crushing [...] Read more.
Soybean-based food products are a major source of protein. In the present study, proteins in soybean milk from seeds of the cultivar Bunya (Glycine max) were extracted using the cheesecloth and the centrifuge methods. The milk was produced through mechanical crushing of both whole and split seeds in water. Following separation by either the cheesecloth or centrifuge, proteins were isolated from the soybean milk by using thiourea/urea solubilisation and then separated them using two-dimensional polyacrylamide gel electrophoresis. The isolated proteins were identified by mass spectrometry. A total of 97 spots were identified including 49 that displayed different abundances. Of the two separation techniques, centrifuge separation gave higher protein extraction and more intense protein spots than cheesecloth separation. Eleven of the β-subunits of β-conglycinin, three of the α-subunits of β-conglycinin, and four of the mutant glycinin showed different levels of abundances between separation techniques, which might be related to subsequent cheese quality. Notably, split-seed soybean milk has less allergenic proteins with four α-subunits of β-conglycinin compared to whole-seed milk with eight of those proteins. The sensory evaluation showed that the cheese produced from split-soybean milk received higher consumer preferences compared to that of whole seed, which could be explained by their proteomic differences. The demonstrated reference map for whole and split-seed soybean milk could be further utilized in the research related to soybean cheesemaking. Full article
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19 pages, 2374 KiB  
Article
Chemical Characterization and Biological Activity of the Mastic Gum Essential Oils of Pistacia lentiscus var. chia from Turkey
by Nurhayat Tabanca, Ayse Nalbantsoy, Paul E. Kendra, Fatih Demirci and Betul Demirci
Molecules 2020, 25(9), 2136; https://doi.org/10.3390/molecules25092136 - 02 May 2020
Cited by 29 | Viewed by 6774
Abstract
The essential oils (EOs) were isolated by hydrodistillation from wild and cultivated Pistacia lentiscus L. var. chia—mastic gum tree (Anacardiaceae) from two natural habitats, namely from Cesme–Uzunkoy (1) and Mordogan (2), and one cultivated source, Cesme–Germiyan (3), in Izmir, Turkey. This comparative [...] Read more.
The essential oils (EOs) were isolated by hydrodistillation from wild and cultivated Pistacia lentiscus L. var. chia—mastic gum tree (Anacardiaceae) from two natural habitats, namely from Cesme–Uzunkoy (1) and Mordogan (2), and one cultivated source, Cesme–Germiyan (3), in Izmir, Turkey. This comparative study evaluated the chemical composition and biological activity of mastic gum essential oils (MGEOs). For this purpose, MGEOs 1–3 were analyzed by gas chromatography–flame ionization detection (GC-FID), gas chromatography–mass spectrometry (GC-MS), and chiral GC for α-pinene. Laboratory assays were conducted to assess for potential in vitro cytotoxicity (multiple in vitro cancer cell lines), antimicrobial properties (five bacterial species and yeast), anti-inflammatory activity (inhibition of inducible nitric oxide synthase, iNOS), and the attraction of Ceratitis capitata (Mediterranean fruit fly, medfly), respectively. Chemical analysis indicated that MGEOs 1 and 2 were rich in α-pinene (56.2% and 51.9%), myrcene (20.1% and 18.6%), and β-pinene (2.7% and 3.1%), respectively; whereas MGEO-3 was characterized by a high level of α-pinene (70.8%), followed by β-pinene (5.7%) and myrcene (2.5%). Chiral GC analyses showed that concentration ratios between (−)/(+)-α-pinene and (−)-α-pinene/myrcene allowed for differentiation between wild and cultivated MGEO sources. In biological assays, MGEOs 1–3 did not exhibit significant antimicrobial effects against the pathogens evaluated and were not strong attractants of male medflies; however, all three MGEOs displayed a dose-dependent inhibition of iNOS, and MGEOs 1 and 2 exhibited selective in vitro cytotoxicity against human cancer cells. These results suggest that wild-type mastic gum oils from Cesme and Mordogan (MGEOs 1 and 2) are potential sources of beneficial products and warrant further investigation. Full article
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17 pages, 760 KiB  
Article
Tuning of the Amount of Se in Rice (Oryza sativa) Grain by Varying the Nature of the Irrigation Method: Development of an ICP-MS Analytical Protocol, Validation and Application to 26 Different Rice Genotypes
by Antonino Spanu, Ilaria Langasco, Massimiliano Valente, Mario Antonello Deroma, Nadia Spano, Francesco Barracu, Maria Itria Pilo and Gavino Sanna
Molecules 2020, 25(8), 1861; https://doi.org/10.3390/molecules25081861 - 17 Apr 2020
Cited by 9 | Viewed by 3093
Abstract
The amount of specific trace elements like selenium (Se) may be of health concern for humans if contained in too high (or low) quantities in staple foods like rice. Among the attempts aimed to optimize the Se concentration in rice, only few studies [...] Read more.
The amount of specific trace elements like selenium (Se) may be of health concern for humans if contained in too high (or low) quantities in staple foods like rice. Among the attempts aimed to optimize the Se concentration in rice, only few studies have been focused on the use of irrigation methods other than continuous flooding. Since intermittent irriguous methods, like sprinkler and saturation, have found to be effective in modifying the bioaccumulation of arsenic and cadmium in rice kernels, the main goal of this study is to measure the amount of the total Se contained in grains of 26 rice genotypes cultivated for two consecutive agrarian vintages in the same open field and with the same water, but differently irrigated with continuous flooding, sprinkler or saturation. To do this, an original and validated ICP-MS method has been developed. The validation parameters accounted for a high sensitivity and accuracy. Sprinkler irrigation is able to reduce in the average of 90% the amount of total Se in kernels in comparison to values measured in rice irrigated with continuous flooding. In conclusion, different irrigation techniques and rice genotypes seem to be valuable tools in order to allow in the future the customized modulation of the Se concentration in rice grain according to the needs of the various populations. Full article
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2019

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14 pages, 5045 KiB  
Article
In Situ Real-Time Tracing of Organophosphorus Pesticides in Apples by Solid-Phase Microextraction with Developed Sampling-Rate Calibration
by Xiao-Fan Zhang, Li-Li Zhao, Ming-Quan Huang, Xiu-Juan Li and Si-Yi Pan
Molecules 2019, 24(24), 4444; https://doi.org/10.3390/molecules24244444 - 04 Dec 2019
Cited by 9 | Viewed by 2528
Abstract
An in situ tracing study based on solid-phase microextraction (SPME) was conducted to investigate the uptake and elimination of organophosphorus pesticides in apples. A matrix-compatible polydimethylsiloxane/poly(styrene-co-divinylbenzene)/polydimethylsiloxane fiber was produced to meet the needs of in situ sampling. The fiber had high extraction ability, [...] Read more.
An in situ tracing study based on solid-phase microextraction (SPME) was conducted to investigate the uptake and elimination of organophosphorus pesticides in apples. A matrix-compatible polydimethylsiloxane/poly(styrene-co-divinylbenzene)/polydimethylsiloxane fiber was produced to meet the needs of in situ sampling. The fiber had high extraction ability, good sensitivity and accuracy with respect to the analytes in apple pulp, and could be used 85 times. Although the sampling rate was changing over time, quantification was still achieved by the sampling rate calibration method. Some factors that affect its applicability were studied. The limits of detection were 0.18 ng/g for diazinon and 0.20 ng/g for chlorpyrifos, rather lower than the maximum residue limits of the National Food Safety Standard of China (GB 2763-2016) and the European Commission (Reg.(EU) No 834/2013, 2018/686). The accuracy of in situ SPME quantification was verified by comparing with the results obtained by the traditional liquid–liquid extraction method. In this work, the in situ sampling method is developed using apples, diazinon, and chlorpyrifos as a model system; however, this method can be used for in vivo analysis of fruits and vegetables for nutrition and safety monitoring. Full article
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14 pages, 1396 KiB  
Article
Correlation Between the Water Solubility and Secondary Structure of Tilapia-Soybean Protein Co-Precipitates
by Li Tan, Pengzhi Hong, Ping Yang, Chunxia Zhou, Dinghao Xiao and Tanjun Zhong
Molecules 2019, 24(23), 4337; https://doi.org/10.3390/molecules24234337 - 27 Nov 2019
Cited by 26 | Viewed by 3318
Abstract
The secondary structure of a protein has been identified to be a crucial indicator that governs its water solubility. Tilapia protein isolate (TPI), soybean protein isolate (SPI), and tilapia-soybean protein co-precipitates (TSPC3:1, TSPC2:1, TSPC1:1, TSPC1:2, [...] Read more.
The secondary structure of a protein has been identified to be a crucial indicator that governs its water solubility. Tilapia protein isolate (TPI), soybean protein isolate (SPI), and tilapia-soybean protein co-precipitates (TSPC3:1, TSPC2:1, TSPC1:1, TSPC1:2, and TSPC1:3) were prepared by mixing tilapia meat and soybean meal at different mass ratios. The results demonstrated that the water solubility of TSPCs was significantly greater than that of TPI (p <0.05). The changes in ultraviolet–visible and near-ultraviolet circular dichroism spectra indicated that the local structure of TSPCs was different from that of TPI and SPI. Fourier transform infrared Spectroscopy revealed the co-existence of TPI and SPI structures in TSPCs. The secondary structures of TSPCs were predominantly α-helix and β-sheet. TSPC1:1 was unique compared to the other TSPCs. In addition, there was a good correlation between the water solubility and secondary structure of TSPCs, in which the correlation coefficients of α-helix and β-sheet were −0.964 (p <0.01) and 0.743, respectively. TSPCs displayed lower α-helix contents and higher β-sheet contents compared to TPI, which resulted in a significant increase in their water solubility. Our findings could provide insight into the structure–function relationship of food proteins, thus creating more opportunities to develop innovative applications for mixed proteins. Full article
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15 pages, 2026 KiB  
Article
Application of Spectroscopic UV-Vis and FT-IR Screening Techniques Coupled with Multivariate Statistical Analysis for Red Wine Authentication: Varietal and Vintage Year Discrimination
by Elisabeta-Irina Geană, Corina Teodora Ciucure, Constantin Apetrei and Victoria Artem
Molecules 2019, 24(22), 4166; https://doi.org/10.3390/molecules24224166 - 17 Nov 2019
Cited by 45 | Viewed by 4750
Abstract
One of the most important issues in the wine sector and prevention of adulterations of wines are discrimination of grape varieties, geographical origin of wine, and year of vintage. In this experimental research study, UV-Vis and FT-IR spectroscopic screening analytical approaches together with [...] Read more.
One of the most important issues in the wine sector and prevention of adulterations of wines are discrimination of grape varieties, geographical origin of wine, and year of vintage. In this experimental research study, UV-Vis and FT-IR spectroscopic screening analytical approaches together with chemometric pattern recognition techniques were applied and compared in addressing two wine authentication problems: discrimination of (i) varietal and (ii) year of vintage of red wines produced in the same oenological region. UV-Vis and FT-IR spectra of red wines were registered for all the samples and the principal features related to chemical composition of the samples were identified. Furthermore, for the discrimination and classification of red wines a multivariate data analysis was developed. Spectral UV-Vis and FT-IR data were reduced to a small number of principal components (PCs) using principal component analysis (PCA) and then partial least squares discriminant analysis (PLS-DA) and linear discriminant analysis (LDA) were performed in order to develop qualitative classification and regression models. The first three PCs used to build the models explained 89% of the total variance in the case of UV-Vis data and 98% of the total variance for FR-IR data. PLS-DA results show that acceptable linear regression fits were observed for the varietal classification of wines based on FT-IR data. According to the obtained LDA classification rates, it can be affirmed that UV-Vis spectroscopy works better than FT-IR spectroscopy for the discrimination of red wines according to the grape variety, while classification of wines according to year of vintage was better for the LDA based FT-IR data model. A clear discrimination of aged wines (over six years) was observed. The proposed methodologies can be used as accessible tools for the wine identity assurance without the need for costly and laborious chemical analysis, which makes them more accessible to many laboratories. Full article
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20 pages, 1979 KiB  
Article
Transfer of a Multiclass Method for over 60 Antibiotics in Food from High Resolution to Low Resolution Mass Spectrometry
by Danilo Giusepponi, Fabiola Paoletti, Carolina Barola, Simone Moretti, Giorgio Saluti, Federica Ianni, Roccaldo Sardella and Roberta Galarini
Molecules 2019, 24(16), 2935; https://doi.org/10.3390/molecules24162935 - 13 Aug 2019
Cited by 7 | Viewed by 3719
Abstract
A multiclass method has been developed to screen and confirm a wide range of anti-microbial residues in muscle and milk, and validated using liquid-chromatography coupled to (low-resolution, LR) tandem mass spectrometry (LC-QqQ). Over sixty antibiotics, belonging to ten distinct families, were included in [...] Read more.
A multiclass method has been developed to screen and confirm a wide range of anti-microbial residues in muscle and milk, and validated using liquid-chromatography coupled to (low-resolution, LR) tandem mass spectrometry (LC-QqQ). Over sixty antibiotics, belonging to ten distinct families, were included in the method scope. The development process was rapidly concluded as a result of two previously implemented methods. This consisted of identical sample treatments, followed by liquid chromatography, and coupled with high-resolution (HR) mass spectrometry (LC-Q-Orbitrap). The validation study was performed in the range between 10–1500 μg·kg−1 for muscles and 2–333 μg·kg−1 for milk. The main performance characteristics were estimated and, then, compared to those previously obtained with HR technique. The validity of the method transfer was ascertained also through inter-laboratory studies. Full article
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28 pages, 2741 KiB  
Review
Ion Mobility Spectrometry in Food Analysis: Principles, Current Applications and Future Trends
by Maykel Hernández-Mesa, David Ropartz, Ana M. García-Campaña, Hélène Rogniaux, Gaud Dervilly-Pinel and Bruno Le Bizec
Molecules 2019, 24(15), 2706; https://doi.org/10.3390/molecules24152706 - 25 Jul 2019
Cited by 122 | Viewed by 9064
Abstract
In the last decade, ion mobility spectrometry (IMS) has reemerged as an analytical separation technique, especially due to the commercialization of ion mobility mass spectrometers. Its applicability has been extended beyond classical applications such as the determination of chemical warfare agents and nowadays [...] Read more.
In the last decade, ion mobility spectrometry (IMS) has reemerged as an analytical separation technique, especially due to the commercialization of ion mobility mass spectrometers. Its applicability has been extended beyond classical applications such as the determination of chemical warfare agents and nowadays it is widely used for the characterization of biomolecules (e.g., proteins, glycans, lipids, etc.) and, more recently, of small molecules (e.g., metabolites, xenobiotics, etc.). Following this trend, the interest in this technique is growing among researchers from different fields including food science. Several advantages are attributed to IMS when integrated in traditional liquid chromatography (LC) and gas chromatography (GC) mass spectrometry (MS) workflows: (1) it improves method selectivity by providing an additional separation dimension that allows the separation of isobaric and isomeric compounds; (2) it increases method sensitivity by isolating the compounds of interest from background noise; (3) and it provides complementary information to mass spectra and retention time, the so-called collision cross section (CCS), so compounds can be identified with more confidence, either in targeted or non-targeted approaches. In this context, the number of applications focused on food analysis has increased exponentially in the last few years. This review provides an overview of the current status of IMS technology and its applicability in different areas of food analysis (i.e., food composition, process control, authentication, adulteration and safety). Full article
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12 pages, 2498 KiB  
Article
Discrimination of Natural Mature Acacia Honey Based on Multi-Physicochemical Parameters Combined with Chemometric Analysis
by Tianchen Ma, Haoan Zhao, Caiyun Liu, Min Zhu, Hui Gao, Ni Cheng and Wei Cao
Molecules 2019, 24(14), 2674; https://doi.org/10.3390/molecules24142674 - 23 Jul 2019
Cited by 14 | Viewed by 3559
Abstract
Honey maturity is an important factor in evaluating the quality of honey. We established a method for the identification of natural mature acacia honey with eighteen physicochemical parameters combined with chemometric analysis. The analysis of variance showed significant differences between mature and immature [...] Read more.
Honey maturity is an important factor in evaluating the quality of honey. We established a method for the identification of natural mature acacia honey with eighteen physicochemical parameters combined with chemometric analysis. The analysis of variance showed significant differences between mature and immature acacia honey in physicochemical parameters. The principal component analysis explained 82.64% of the variance among samples, and indicated that total phenolic content, total protein content, and total sugar (glucose, fructose, sucrose) were the major variables. The cluster analysis and orthogonal partial least squares-discriminant analysis demonstrated that samples were grouped in relation to the maturity coinciding with the results of the principal component analysis. Meanwhile, the 35 test samples were classified with 100% accuracy with the method of multi-physicochemical parameters combined with chemometric analysis. All the results presented above proved the possibility of identifying mature acacia honey and immature acacia honey according to the chemometric analysis based on the multi-physicochemical parameters. Full article
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11 pages, 1411 KiB  
Article
Use of 1H NMR to Detect the Percentage of Pure Fruit Juices in Blends
by Lucia Marchetti, Federica Pellati, Stefania Benvenuti and Davide Bertelli
Molecules 2019, 24(14), 2592; https://doi.org/10.3390/molecules24142592 - 17 Jul 2019
Cited by 20 | Viewed by 3484
Abstract
The consumption of high-nutritional-value juice blends is increasing worldwide and, considering the large market volume, fraud and adulteration represent an ongoing problem. Therefore, advanced anti-fraud tools are needed. This study aims to verify the potential of 1H NMR combined with partial least [...] Read more.
The consumption of high-nutritional-value juice blends is increasing worldwide and, considering the large market volume, fraud and adulteration represent an ongoing problem. Therefore, advanced anti-fraud tools are needed. This study aims to verify the potential of 1H NMR combined with partial least squares regression (PLS) to determine the relative percentage of pure fruit juices in commercial blends. Apple, orange, pineapple, and pomegranate juices were selected to set up an experimental plan and then mixed in different proportions according to a central composite design (CCD). NOESY (nuclear Overhauser enhancement spectroscopy) experiments that suppress the water signal were used. Considering the high complexity of the spectra, it was necessary to pretreat and then analyze by chemometric tools the large amount of information contained in the raw data. PLS analysis was performed using venetian-blind internal cross-validation, and the model was established using different chemometric indicators (RMSEC, RMSECV, RMSEP, R2CAL, R2CV, R2PRED). PLS produced the best model, using five factors explaining 94.51 and 88.62% of the total variance in X and Y, respectively. The present work shows the feasibility and advantages of using 1H NMR spectral data in combination with multivariate analysis to develop and optimize calibration models potentially useful for detecting fruit juice adulteration. Full article
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14 pages, 3254 KiB  
Article
Extraction of Carotenoids and Fat-Soluble Vitamins from Tetradesmus Obliquus Microalgae: An Optimized Approach by Using Supercritical CO2
by Laura Chronopoulou, Chiara Dal Bosco, Fabrizio Di Caprio, Letizia Prosini, Alessandra Gentili, Francesca Pagnanelli and Cleofe Palocci
Molecules 2019, 24(14), 2581; https://doi.org/10.3390/molecules24142581 - 16 Jul 2019
Cited by 29 | Viewed by 4669
Abstract
In recent years, great attention has been focused on rapid, selective, and environmentally friendly extraction methods to recover pigments and antioxidants from microalgae. Among these, supercritical fluid extraction (SFE) represents one of the most important alternatives to traditional extraction methods carried out with [...] Read more.
In recent years, great attention has been focused on rapid, selective, and environmentally friendly extraction methods to recover pigments and antioxidants from microalgae. Among these, supercritical fluid extraction (SFE) represents one of the most important alternatives to traditional extraction methods carried out with the use of organic solvents. In this study, the influence of parameters such as pressure, temperature, and the addition of a polar co-solvent in the SFE yields of carotenoids and fat-soluble vitamins from T. obliquus biomass were evaluated. The highest extraction of alpha-tocopherol, gamma-tocopherol, and retinol was achieved at a pressure of 30 MPa and a temperature of 40 °C. It was observed that overall, the extraction yield increased considerably when a preliminary step of sample pre-treatment, based on a matrix solid phase dispersion, was applied using diatomaceous earth as a dispersing agent. The use of ethanol as a co-solvent, under certain conditions of pressure and temperature, resulted in selectively increasing the yields of only some compounds. In particular, a remarkable selectivity was observed if the extraction was carried out in the presence of ethanol at 10 MPa and 40 °C: under these conditions, it was possible to isolate menaquinone-7, a homologous of vitamin K2, which, otherwise, cannot not recovered by using traditional extraction procedures. Full article
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18 pages, 2885 KiB  
Article
Simultaneous Characterization and Quantification of Varied Ingredients from Sojae semen praeparatum in Fermentation Using UFLC–TripleTOF MS
by Chuan Chai, Xiaobing Cui, Chenxiao Shan, Sheng Yu, Xinzhi Wang and Hongmei Wen
Molecules 2019, 24(10), 1864; https://doi.org/10.3390/molecules24101864 - 15 May 2019
Cited by 11 | Viewed by 2843
Abstract
Systematic comparison of active ingredients in Sojae semen praeparatum (SSP) during fermentation was performed using ultra-fast liquid chromatography (UFLC)–TripleTOF MS and principal component analysis (PCA). By using this strategy, a total of 25 varied compounds from various biosynthetic groups were assigned and relatively [...] Read more.
Systematic comparison of active ingredients in Sojae semen praeparatum (SSP) during fermentation was performed using ultra-fast liquid chromatography (UFLC)–TripleTOF MS and principal component analysis (PCA). By using this strategy, a total of 25 varied compounds from various biosynthetic groups were assigned and relatively quantified in the positive or negative ion mode, including two oligosaccharides, twelve isoflavones, eight fatty acids, N–(3–Indolylacetyl)–dl–aspartic acid, methylarginine, and sorbitol. Additionally, as the representative constituents, six targeted isoflavones were sought in a targeted manner and accurately quantified using extracted ion chromatograms (XIC) manager (AB SCIEX, Los Angeles, CA, USA) combined with MultiQuant software (AB SCIEX, Los Angeles, CA, USA). During the fermentation process, the relative contents of oligoses decreased gradually, while the fatty acids increased. Furthermore, the accurate contents of isoflavone glycosides decreased, while aglycones increased and reached a maximum in eight days, which indicated that the ingredients converted obviously and regularly throughout the SSP fermentation. In combination with the morphological changes, which meet the requirements of China Pharmacopoeia, this work suggested that eight days is the optimal time for fermentation of SSP from the aspects of morphology and content. Full article
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16 pages, 2030 KiB  
Article
Development of an Accelerated Solvent Extraction-Ultra-Performance Liquid Chromatography-Fluorescence Detection Method for Quantitative Analysis of Thiamphenicol, Florfenicol and Florfenicol Amine in Poultry Eggs
by Bo Wang, Xing Xie, Xia Zhao, Kaizhou Xie, Zhixiang Diao, Genxi Zhang, Tao Zhang and Guojun Dai
Molecules 2019, 24(9), 1830; https://doi.org/10.3390/molecules24091830 - 13 May 2019
Cited by 8 | Viewed by 3347
Abstract
A simple, rapid and novel method for the detection of residues of thiamphenicol (TAP), florfenicol (FF) and its metabolite, florfenicol amine (FFA), in poultry eggs by ultra-performance liquid chromatography-fluorescence detection (UPLC-FLD) was developed. The samples were extracted with acetonitrile-ammonia (98:2, v/v) using [...] Read more.
A simple, rapid and novel method for the detection of residues of thiamphenicol (TAP), florfenicol (FF) and its metabolite, florfenicol amine (FFA), in poultry eggs by ultra-performance liquid chromatography-fluorescence detection (UPLC-FLD) was developed. The samples were extracted with acetonitrile-ammonia (98:2, v/v) using accelerated solvent extraction (ASE) and purified by manual degreasing with acetonitrile-saturated n-hexane. The target compounds were separated on an ACQUITY UPLC® BEH C18 (2.1 mm × 100 mm, 1.7 μm) chromatographic column using a mobile phase composed of 0.005 mol/L NaH2PO4, 0.003 mol/L sodium lauryl sulfate and 0.05% trimethylamine, adjusted to pH 5.3 ± 0.1 by phosphoric acid and acetonitrile (64:36, v/v). The limits of detection (LODs) and limits of quantification (LOQs) of the three target compounds in poultry eggs were 1.8–4.9 µg/kg and 4.3–11.7 µg/kg, respectively. The recoveries of the three target compounds in poultry eggs were above 80.1% when the spiked concentrations of three phenicols were the LOQ, 0.5 maximum residue limit (MRL), 1.0 MRL and 2.0 MRL. The intraday relative standard deviations (RSDs) were less than 5.5%, and the interday RSDs were less than 6.6%. Finally, this new detection method was successfully applied to the quantitative analysis of TAP, FF and FFA in 150 commercial poultry eggs. Full article
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13 pages, 1052 KiB  
Article
1H-NMR Profiling and Carbon Isotope Discrimination as Tools for the Comparative Assessment of Walnut (Juglans regia L.) Cultivars with Various Geographical and Genetic Origins—A Preliminary Study
by Raluca Popescu, Roxana Elena Ionete, Oana Romina Botoran, Diana Costinel, Felicia Bucura, Elisabeta Irina Geana, Yazan Falah Jadee ’Alabedallat and Mihai Botu
Molecules 2019, 24(7), 1378; https://doi.org/10.3390/molecules24071378 - 08 Apr 2019
Cited by 16 | Viewed by 2825
Abstract
The aim of the study was to investigate the differences between walnut genotypes of various geographical and genetic origins grown under the same or different environmental conditions. The biological material analyzed consisted in walnut kernels of 34 cultivars, nine advanced selections, and six [...] Read more.
The aim of the study was to investigate the differences between walnut genotypes of various geographical and genetic origins grown under the same or different environmental conditions. The biological material analyzed consisted in walnut kernels of 34 cultivars, nine advanced selections, and six hybrids harvested in 2015 and 2016, summing up to a total of 64 samples. The walnuts, walnut oil, and residue were characterized in respect to their chemical (proximate composition—fat, protein, nutritional value, fatty acids profile by 1H-NMR) and carbon-13 isotopic composition. The data was used to statistically discriminate the cultivars according to composition, geographical area of origin, and year of harvest, comparing the Romanian cultivars, selections, and hybrids with the internationally available ones. Full article
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15 pages, 565 KiB  
Article
Chemical Composition, Antioxidant and Antihyperglycemic Activities of the Wild Lactarius deliciosus from China
by Zhou Xu, Liang Fu, Shiling Feng, Ming Yuan, Yan Huang, Jinqiu Liao, Lijun Zhou, Hongyu Yang and Chunbang Ding
Molecules 2019, 24(7), 1357; https://doi.org/10.3390/molecules24071357 - 06 Apr 2019
Cited by 37 | Viewed by 4539
Abstract
The wild mushroom Lactarius deliciosus from China was studied for the first time to obtain information about its chemical composition, antioxidant, and antihyperglycemic activities. Nutritional value, dietary fiber, fatty acids, metal elements, free sugars, free amino acids, organic acids, flavor 5′-nucleotides, and volatile [...] Read more.
The wild mushroom Lactarius deliciosus from China was studied for the first time to obtain information about its chemical composition, antioxidant, and antihyperglycemic activities. Nutritional value, dietary fiber, fatty acids, metal elements, free sugars, free amino acids, organic acids, flavor 5′-nucleotides, and volatile aroma compounds were determined. Potential antioxidant and antihyperglycemic activities were also tested by investigating 1,1-diphenyl-2-picrylhydrazyl (DPPH) and 2,2′-Azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) radicals scavenging activities, ferric ion reducing activity, as well as α-amylase and α-glucosidase inhibitory activities using ethanol and aqueous extracts. The results showed that L. deliciosus was a good wild mushroom with high protein, carbohydrate, and dietary fiber contents, while low in fat and calorie, extensive unsaturated fatty acids contents, with negligible health risks about harmful metal elements. Twenty kinds of free amino acids were detected with a total content 3389.45 mg per 100 g dw. Flavor 5′-nucleotides including 5′-CMP, 5′-UMP, 5′-IMP, and 5′-AMP were 929.85, 45.21, 311.75, and 14.49 mg per 100 g dw, respectively. Mannitol (7825.00 mg per 100 g dw) was the main free sugar, and quininic acid (729.84 mg per 100 g dw) was the main organic acid. Twenty-five kinds of volatile aroma compounds were identified, acids (84.23%) were the most abundant compounds based on content, while aldehydes (15 of 25) were the most abundant compounds based on variety. In addition, both ethanol and aqueous extracts from L. deliciosus exhibited excellent antioxidant activity. While in antihyperglycemic activity tests, only ethanol extracts showed inhibitory effects on α-amylase and α-glucosidase. Full article
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16 pages, 3145 KiB  
Article
A UHPLC-UV Method Development and Validation for Determining Kavalactones and Flavokavains in Piper methysticum (Kava)
by Yijin Tang and Christine Fields
Molecules 2019, 24(7), 1245; https://doi.org/10.3390/molecules24071245 - 30 Mar 2019
Cited by 13 | Viewed by 3900
Abstract
An ultra-high-performance liquid chromatographic (UHPLC) separation was developed for six kava pyrones (methysticin, dihydromethysticin (DHM), kavain, dihydrokavain (DHK), desmethoxyyangonin (DMY), and yangonin), two unidentified components, and three Flavokavains (Flavokavain A, B, and C) in Piper methysticum (kava). The six major kavalactones and three [...] Read more.
An ultra-high-performance liquid chromatographic (UHPLC) separation was developed for six kava pyrones (methysticin, dihydromethysticin (DHM), kavain, dihydrokavain (DHK), desmethoxyyangonin (DMY), and yangonin), two unidentified components, and three Flavokavains (Flavokavain A, B, and C) in Piper methysticum (kava). The six major kavalactones and three flavokavains are completely separated (Rs > 1.5) within 15 min using a HSS T3 column and a mobile phase at 60 °C. All the peaks in the LC chromatogram of kava extract or standard solutions were structurally confirmed by LC-UV-MS/MS. The degradations of yangonin and flavokavains were observed among the method development. The degradation products were identified as cis-isomerization by MS/MS spectra. The isomerization was prevented or limited by sample preparation in a non-alcoholic solvent or with no water. The method uses the six kava pyrones and three flavokavains as external standards. The quantitative calibration curves are linear, covering a range of 0.5–75 μg/mL for the six kava pyrones and 0.05–7.5 μg/mL for the three flavokavains. The quantitation limits for methysticin, DHM, kavain, DHK, DMY, and yangonin are approximately 0.454, 0.480, 0.277, 0.686, 0.189, and 0.422 μg/mL. The limit of quantification (LOQs) of the three flavokavains are about 0.270, 0.062, and 0.303 μg/mL for flavokavain C (FKC), flavokavain A (FKA), and flavokavain B (FKB). The average recoveries at three different levels are 99.0–102.3% for kavalactones (KLs) and 98.1–102.9% for flavokavains (FKs). This study demonstrates that the method of analysis offers convenience and adequate sensitivity for determining methysticin, DHM, kavain, DHK, yangonin, DMY, FKA, FKB, and FKC in kava raw materials (root and CO2 extract) and finished products (dry-filled capsule and tablet). Full article
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17 pages, 1062 KiB  
Review
Analysis of Enantiomers in Products of Food Interest
by Chiara Fanali, Giovanni D’Orazio, Alessandra Gentili and Salvatore Fanali
Molecules 2019, 24(6), 1119; https://doi.org/10.3390/molecules24061119 - 21 Mar 2019
Cited by 39 | Viewed by 4459
Abstract
The separation of enantiomers has been started in the past and continues to be a topic of great interest in various fields of research, mainly because these compounds could be involved in biological processes such as, for example, those related to human health. [...] Read more.
The separation of enantiomers has been started in the past and continues to be a topic of great interest in various fields of research, mainly because these compounds could be involved in biological processes such as, for example, those related to human health. Great attention has been devoted to studies for the analysis of enantiomers present in food products in order to assess authenticity and safety. The separation of these compounds can be carried out utilizing analytical techniques such as gas chromatography, high-performance liquid chromatography, supercritical fluid chromatography, and other methods. The separation is performed mainly employing chromatographic columns containing particles modified with chiral selectors (CS). Among the CS used, modified polysaccharides, glycopeptide antibiotics, and cyclodextrins are currently applied. Full article
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12 pages, 2088 KiB  
Article
Development of an Impedimetric Aptasensor for Label Free Detection of Patulin in Apple Juice
by Reem Khan, Sondes Ben Aissa, Tauqir A. Sherazi, Gaelle Catanante, Akhtar Hayat and Jean Louis Marty
Molecules 2019, 24(6), 1017; https://doi.org/10.3390/molecules24061017 - 13 Mar 2019
Cited by 39 | Viewed by 5585
Abstract
In the present work, an aptasensing platform was developed for the detection of a carcinogenic mycotoxin termed patulin (PAT) using a label-free approach. The detection was mainly based on a specific interaction of an aptamer immobilized on carbon-based electrode. A long linear spacer [...] Read more.
In the present work, an aptasensing platform was developed for the detection of a carcinogenic mycotoxin termed patulin (PAT) using a label-free approach. The detection was mainly based on a specific interaction of an aptamer immobilized on carbon-based electrode. A long linear spacer of carboxy-amine polyethylene glycol chain (PEG) was chemically grafted on screen-printed carbon electrodes (SPCEs) via diazonium salt in the aptasensor design. The NH2-modified aptamer was then attached covalently to carboxylic acid groups of previously immobilized bifunctional PEG to build a diblock macromolecule. The immobilized diblocked molecules resulted in the formation of long tunnels on a carbon interface, while the aptamer was assumed as the gate of these tunnels. Upon target analyte binding, the gates were assumed to be closed due to conformational changes in the structure of the aptamer, increasing the resistance to the charge transfer. This increase in resistance was measured by electrochemical impedance spectroscopy, the main analytical technique for the quantitative detection of PAT. Encouragingly, a good linear range between 1 and 25 ng was obtained. The limit of detection and limit of quantification was 2.8 ng L−1 and 4.0 ng L−1, respectively. Selectivity of the aptasensor was confirmed with mycotoxins commonly occurring in food. The developed apta-assay was also applied to a real sample, i.e., fresh apple juice spiked with PAT, and toxin recovery up to 99% was observed. The results obtained validated the suitability and selectivity of the developed apta-assay for the identification and quantification of PAT in real food samples. Full article
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16 pages, 1925 KiB  
Article
Fatty Acid, Lipid Classes and Phospholipid Molecular Species Composition of the Marine Clam Meretrix lyrata (Sowerby 1851) from Cua Lo Beach, Nghe An Province, Vietnam
by Quoc Toan Tran, Thi Thanh Tra Le, Minh Quan Pham, Tien Lam Do, Manh Hung Vu, Duy Chinh Nguyen, Long Giang Bach, Le Minh Bui and Quoc Long Pham
Molecules 2019, 24(5), 895; https://doi.org/10.3390/molecules24050895 - 04 Mar 2019
Cited by 28 | Viewed by 4557
Abstract
This study aims to analyze compositions of fatty acids and phospholipid molecular species in the hard clams Meretrix lyrata (Sowerby, 1851) harvested from Cua Lo beach, Nghe An province, Viet Nam. Total lipid of hard clams Meretrix lyrata occupied 1.7 ± 0.2% of [...] Read more.
This study aims to analyze compositions of fatty acids and phospholipid molecular species in the hard clams Meretrix lyrata (Sowerby, 1851) harvested from Cua Lo beach, Nghe An province, Viet Nam. Total lipid of hard clams Meretrix lyrata occupied 1.7 ± 0.2% of wet weight and contained six classes: hydrocarbon and wax (HW), triacylglycerol (TAG), free fatty acids (FFA), sterol (ST), polar lipid (PoL), and monoalkyl diacylglycerol (MADAG). Among the constituents, the proportion of PoL accounted was highest, at 45.7%. In contrast, the figures for MADAG were lowest, at 1.3%. Twenty-six fatty acids were identified with the ratios of USAFA/SAFA was 2. The percentage of n-3 PUFA (ω-3) and n-6 PUFA (ω-6) was high, occupying 38.4% of total FA. Among PUFAs, arachidonic acid (AA, 20:4n-6), eicosapentaenoic acid (EPA, 20:5n-3), docosapentaenoic acid (DPA, 22:5n-3), and docosahexaenoic acid (DHA, 22:6n-3) accounted for 3.8%, 7.8%, 2.2% and 12.0% of total lipid of the clam respectively. Phospholipid molecular species were identified in polar lipids of the clams consisting six types: phosphatidylethalnolamine (PE, with 28 molecular species), phosphatidylcholine (PC, with 26 molecular species), phosphatidylserine (PS, with 18 molecular species), phosphatidylinositol (PI, with 10 molecular species), phosphatidylglycerol (PG, with only one molecular species), and ceramide aminoethylphosphonate (CAEP, with 15 molecular species). This is the first time that the molecular species of sphingophospholipid were determined, in Meretrix lyrata in particular, and for clams in general. Phospholipid formula species of PE and PS were revealed to comprise two kinds: Alkenyl acyl glycerophosphoethanolamine and Alkenyl acyl glycerophosphoserine occupy 80.3% and 81.0% of total PE and PS species, respectively. In contrast, the percentage of diacyl glycero phosphatidylcholine was twice as high as that of PakCho in total PC, at 69.3, in comparison with 30.7%. In addition, phospholipid formula species of PI and PG comprised only diacyl glycoro phospholipids. PE 36:1 (p18:0/18:1), PC 38:6 (16:0/22:6), PS 38:1 (p18:0/20:1), PI 40:5 (20:1/20:4), PG 32:0 (16:0/16:0) and CAEP 34:2 (16:2/d18:0) were the major molecular species. Full article
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16 pages, 5187 KiB  
Article
Morphology and Molecular Identification of Twelve Commercial Varieties of Kiwifruit
by Qiaoli Xie, Hongbo Zhang, Fei Yan, Chunxia Yan, Shuguang Wei, Jianghua Lai, Yunpeng Wang and Bao Zhang
Molecules 2019, 24(5), 888; https://doi.org/10.3390/molecules24050888 - 03 Mar 2019
Cited by 13 | Viewed by 3856
Abstract
The quality and safety of food are important guarantees for the health and legal rights of consumers. As an important special fruitcrop, there are frequently shoddy practices in the kiwifruit (Actinidia chinensis) market, which harms the interests of consumers. However, there [...] Read more.
The quality and safety of food are important guarantees for the health and legal rights of consumers. As an important special fruitcrop, there are frequently shoddy practices in the kiwifruit (Actinidia chinensis) market, which harms the interests of consumers. However, there is lack of rapid and accurate identification methods for commercial kiwifruit varieties. Here, twelve common commercial varieties of kiwifruit were morphologically discriminated. DNA barcodes of chloroplast regions psbA-trnH, rbcL, matK, rpoB, rpoC1, ycf1b, trnL and rpl32_trnL(UAG), the nuclear region At103 and intergenic region ITS2 were amplified. Divergences and phylogenetic trees were used to analyze the phylogenetic relationship of these twelve commercial kiwifruit varieties. The results showed that matK, ITS2 and rpl32_trnL(UAG) can be utilized as molecular markers to identify CuiYu, JinYan, HuangJinGuo, ChuanHuangJin, HuaYou, YaTe, XuXiang and HongYang. This provides experimental and practical basis to scientifically resolve kiwifruit-related judicial disputes and legal trials. Full article
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21 pages, 2886 KiB  
Article
Alternative Ultrasound-Assisted Method for the Extraction of the Bioactive Compounds Present in Myrtle (Myrtus communis L.)
by Ana V. González de Peredo, Mercedes Vázquez-Espinosa, Estrella Espada-Bellido, Marta Ferreiro-González, Antonio Amores-Arrocha, Miguel Palma, Gerardo F. Barbero and Ana Jiménez-Cantizano
Molecules 2019, 24(5), 882; https://doi.org/10.3390/molecules24050882 - 02 Mar 2019
Cited by 32 | Viewed by 3916
Abstract
The bioactive compounds in myrtle berries, such as phenolic compounds and anthocyanins, have shown a potentially positive effect on human health. Efficient extraction methods are to be used to obtain maximum amounts of such beneficial compounds from myrtle. For that reason, this study [...] Read more.
The bioactive compounds in myrtle berries, such as phenolic compounds and anthocyanins, have shown a potentially positive effect on human health. Efficient extraction methods are to be used to obtain maximum amounts of such beneficial compounds from myrtle. For that reason, this study evaluates the effectiveness of a rapid ultrasound-assisted method (UAE) to extract anthocyanins and phenolic compounds from myrtle berries. The influence of solvent composition, as well as pH, temperature, ultrasound amplitude, cycle and solvent-sample ratio on the total phenolic compounds and anthocyanins content in the extracts obtained were evaluated. The response variables were optimized by means of a Box-Behnken design. It was found that the double interaction of the methanol composition and the cycle, the interaction between methanol composition and temperature, and the interaction between the cycle and solvent-sample ratio were the most influential variables on the extraction of total phenolic compounds (92.8% methanol in water, 0.2 s of cycle, 60 °C and 10:0.5 mL:g). The methanol composition and the interaction between methanol composition and pH were the most influential variables on the extraction of anthocyanins (74.1% methanol in water at pH 7). The methods that have been developed presented high repeatability and intermediate precision (RSD < 5%) and the bioactive compounds show a high recovery with short extraction times. Both methods were used to analyze the composition of the bioactive compounds in myrtle berries collected from different locations in the province of Cadiz (Spain). The results obtained by UAE were compared to those achieved in a previous study where microwave-assisted extraction (MAE) methods were employed. Similar extraction yields were obtained for phenolic compounds and anthocyanins by MAE and UAE under optimal conditions. However, UAE presents the advantage of using milder conditions for the extraction of anthocyanins from myrtle, which makes of this a more suitable method for the extraction of these degradable compounds. Full article
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13 pages, 3373 KiB  
Article
Flavor Profile Evolution of Bottle Aged Rosé and White Wines Sealed with Different Closures
by Meng-Qi Ling, Han Xie, Yu-Bo Hua, Jian Cai, Si-Yu Li, Yi-Bin Lan, Ruo-Nan Li, Chang-Qing Duan and Ying Shi
Molecules 2019, 24(5), 836; https://doi.org/10.3390/molecules24050836 - 27 Feb 2019
Cited by 7 | Viewed by 3169
Abstract
Bottle aging is the final stage before wines are drunk, and is considered as a maturation time when many chemical changes occur. To get a better understanding of the evolution of wines’ flavor profile, the flavor compounds (phenolic and volatile compounds), dissolved oxygen [...] Read more.
Bottle aging is the final stage before wines are drunk, and is considered as a maturation time when many chemical changes occur. To get a better understanding of the evolution of wines’ flavor profile, the flavor compounds (phenolic and volatile compounds), dissolved oxygen (DO), and flavor characters (OAVs and chromatic parameters) of rosé and dry white wines bottled with different closures were determined after 18 months’ bottle aging. The results showed the main phenolic change trends of rosé wines were decreasing while the trends of white wines were increasing, which could be the reason for their unique DO changing behaviors. Volatile compounds could be clustered into fluctuating, increasing, and decreasing groups using k-means algorithm. Most volatile compounds, especially some long-chain aliphatic acid esters (octanoates and decanoates), exhibited a lower decrease rate in rosé wines sealed with natural corks and white wines with screw caps. After 18 months of bottle aging, wines treated with natural corks and their alternatives could be distinguished into two groups based on flavor compounds via PLS-DA. As for flavor characters, the total intensity of aroma declined obviously compared with their initial counterparts. Rosé wines exhibit visual difference in color, whereas such a phenomenon was not observed in white wines. Full article
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21 pages, 4461 KiB  
Article
Analysis of 27 β-Blockers and Metabolites in Milk Powder by High Performance Liquid Chromatography Coupled to Quadrupole Orbitrap High-Resolution Mass Spectrometry
by Jian-Qiao Cheng, Tong Liu, Xue-Mei Nie, Feng-Ming Chen, Chuan-Sheng Wang and Feng Zhang
Molecules 2019, 24(4), 820; https://doi.org/10.3390/molecules24040820 - 25 Feb 2019
Cited by 14 | Viewed by 3635
Abstract
This paper presents an application of high performance liquid chromatography coupled with quadrupole orbitrap high-resolution mass spectrometry (HPLC-Q-Orbitrap HRMS) for the analysis of 27 β-blockers and metabolites in milk powder. Homogenized milk power samples were extracted by acetonitrile and purified by using Oasis [...] Read more.
This paper presents an application of high performance liquid chromatography coupled with quadrupole orbitrap high-resolution mass spectrometry (HPLC-Q-Orbitrap HRMS) for the analysis of 27 β-blockers and metabolites in milk powder. Homogenized milk power samples were extracted by acetonitrile and purified by using Oasis PRiME HLB solid-phase extraction cartridges. The Ascentis® C8 chromatographic column was used to separate the analytes. The quantification was achieved by using matrix-matched standard calibration curves with carazolol-d7 and propranolol-d7 as the internal standards. The results show an exceptional linear relationship with the concentrations of analytes over wide concentration ranges (0.5–500 μg kg−1) as all the fitting coefficients of determination r2 are > 0.995. All the limits of detection (LODs) and quantitation (LOQs) values were within the respective range of 0.2–1.5 μg kg−1 and 0.5–5.0 μg kg−1. Overall average recoveries were able to reach 66.1–100.4% with the intra- and inter-day variability under 10%. This method has been successfully applied to the screening of β-blockers and metabolites in commercial milk powders. At the same time, the corresponding characteristic fragmentation behavior of the 27 compounds was explored. The characteristic product ions were determined and applied to the actual samples screening. Full article
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12 pages, 2315 KiB  
Article
Identification of the Pol Gene as a Species-Specific Diagnostic Marker for Qualitative and Quantitative PCR Detection of Tricholoma matsutake
by Luying Shan, Dazhou Wang, Yinjiao Li, Shi Zheng, Wentao Xu and Ying Shang
Molecules 2019, 24(3), 455; https://doi.org/10.3390/molecules24030455 - 28 Jan 2019
Cited by 4 | Viewed by 3215
Abstract
Tricholoma matsutake is a rare, precious, and wild edible fungus that could not be cultivated artificially until now. This situation has given way to the introduction of fake T. matsutake commodities to the mushroom market. Among the methods used to detect food adulteration, [...] Read more.
Tricholoma matsutake is a rare, precious, and wild edible fungus that could not be cultivated artificially until now. This situation has given way to the introduction of fake T. matsutake commodities to the mushroom market. Among the methods used to detect food adulteration, amplification of species-specific diagnostic marker is particularly important and accurate. In this study, the Pol gene is reported as a species-specific diagnostic marker to identify three T. matsutake varieties and 10 other types of edible mushrooms through qualitative and quantitative PCR. The PCR results did not reveal variations in the amplified region, and the detection limits of qualitative and quantitative PCR were found to be 8 ng and 32 pg, respectively. Southern blot showed that the Pol gene exists as a single copy in the T. matsutake genome. The method that produced the purest DNA of T. matsutake in this study was also determined, and the high-concentration salt precipitation method was confirmed to be the most suitable among the methods tested. The assay proposed in this work is applicable not only to the detection of raw materials but also to the examination of processed products containing T. matsutake. Full article
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2018

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12 pages, 759 KiB  
Article
Small Molecular Weight Aldose (d-Glucose) and Basic Amino Acids (l-Lysine, l-Arginine) Increase the Occurrence of PAHs in Grilled Pork Sausages
by Wen Nie, Ke-zhou Cai, Yu-zhu Li, Shuo Zhang, Yu Wang, Jie Guo, Cong-gui Chen and Bao-cai Xu
Molecules 2018, 23(12), 3377; https://doi.org/10.3390/molecules23123377 - 19 Dec 2018
Cited by 22 | Viewed by 3767
Abstract
(1) Background: Amino acids and carbohydrates are widely used as additives in the food industry. These compounds have been proven to be an influencing factor in the production of chemical carcinogenic compounds polycyclic aromatic hydrocarbons (PAHs). However, the effect of the properties of [...] Read more.
(1) Background: Amino acids and carbohydrates are widely used as additives in the food industry. These compounds have been proven to be an influencing factor in the production of chemical carcinogenic compounds polycyclic aromatic hydrocarbons (PAHs). However, the effect of the properties of the amino acids and carbohydrates on the production of PAHs is still little known. (2) Methods: We added different (i) R groups (the R group represents an aldehyde group in a glucose molecule or a ketone group in a fructose molecule); (ii) molecular weight carbohydrates; (iii) polarities, and (iv) acid-base amino acids to pork sausages. The effects of the molecular properties of carbohydrates and amino acids on the formation of PAHs in grilled pork sausages were investigated. (3) Results: The results showed that a grilled sausage with aldehyde-based d-glucose was capable of producing more PAHs than a sausage with keto-based d-fructose. A higher PAH content was determined in the grilled pork sausage when the smaller molecular weight, d-glucose, was added compared with the sausage where the larger molecular weight, 4-(α-d-glucosido)-d-glucose and cellulose were added. The addition of basic amino acids (l-lysine, l-arginine) was capable of producing more PAHs compared with the addition of acidic amino acids (l-glutamic acid, l-aspartate). When amino acid containing a benzene ring was added, a smaller volume of PAHs was produced compared with the addition of other amino acids. (4) Conclusions: Our study suggests that systematic consideration of molecule properties is necessary when using food additives (amino acids and carbohydrates) for food processing. Full article
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17 pages, 1726 KiB  
Article
Spectrum-Effect Relationships between High-Performance Liquid Chromatography (HPLC) Fingerprints and the Antioxidant and Anti-Inflammatory Activities of Collagen Peptides
by Junwen Wang, Dan Luo, Ming Liang, Ting Zhang, Xiquan Yin, Ying Zhang, Xiangliang Yang and Wei Liu
Molecules 2018, 23(12), 3257; https://doi.org/10.3390/molecules23123257 - 10 Dec 2018
Cited by 31 | Viewed by 5858
Abstract
A total of 13 batches of collagen peptide samples were extracted, isolated, and purified from chicken sternal cartilage under various process parameters. The fingerprint profiles of 13 batches of collagen peptides were established by high-performance liquid chromatography (HPLC). In addition, the amino acid [...] Read more.
A total of 13 batches of collagen peptide samples were extracted, isolated, and purified from chicken sternal cartilage under various process parameters. The fingerprint profiles of 13 batches of collagen peptides were established by high-performance liquid chromatography (HPLC). In addition, the amino acid profiles and molecular weight distributions of collagen peptides were investigated. The in vitro antioxidant activities of the peptide samples were measured using the 2,2′-Azinobis (3-ethylbenzothiazoline-6-sulphonic acid) diammonium salt (ABTS) assay, the 2,2-diphenyl-1-picrylhydrazyl (DPPH) assay, the ferric-reducing antioxidant power (FRAP) assay and an assay of the oxidative damage induced by hydrogen peroxide (H2O2) in the degenerative cartilage cells from the knee joint of rat C518 (C518 cell line). The anti-inflammatory activities of the peptide samples were assessed by measuring the inflammatory responses induced by lipopolysaccharides (LPS) in C518 cells. Subsequently, the spectrum-effect relationships between HPLC fingerprints and the antioxidant and anti-inflammatory activities of collagen peptides were investigated using grey relational analysis (GRA). Fifteen common peaks were obtained from the HPLC fingerprints of collagen peptides. Each collagen peptide sample had a characteristic set of amino acid types and contents. All of the hydrolysates of the collagen peptides were primarily composed of fractions II (500–1000 Da) and III (1000–3000 Da). Collagen peptides exhibited good scavenging activity on ABTS radical, DPPH radical, and ferric-reducing antioxidant power. Collagen peptides were also effective against H2O2-induced cellular oxidative damage in C518 cells. The antioxidant activity of collagen peptides was due to the low molecular weight and the presence of antioxidant and hydrophobic amino acid residues within its sequence. Collagen peptides significantly inhibited the secretion of inflammatory cytokines IL-1β, TNF-α, and PGE2 in C518 cells. The anti-inflammatory activity of collagen peptides may include increased synthesis of the key components of extracellular matrix (ECM) and inhibited apoptosis of chondrocytes. The GRA results showed that peaks 2, 3, and 8 were the main components contributing to the antioxidant activity of the collagen peptides, whereas peaks 11 and 14 were the main components contributing to the anti-inflammatory activity of the collagen peptides. The components of peaks 8 and 14 were identified as GPRGPPGPVGP and VAIQAVLSLYASGR by UPLC-MS/MS. Those identified collagen peptides offer a potential therapeutic strategy for the treatment of osteoarthritis (OA) due to their antioxidative stress and due to them disturbing the catabolism and anabolism processes in arthrodial cartilage. Full article
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16 pages, 903 KiB  
Article
Phytochemical and Biological Characteristics of Mexican Chia Seed Oil
by Yingbin Shen, Liyou Zheng, Jun Jin, Xiaojing Li, Junning Fu, Mingzhong Wang, Yifu Guan and Xun Song
Molecules 2018, 23(12), 3219; https://doi.org/10.3390/molecules23123219 - 06 Dec 2018
Cited by 47 | Viewed by 4892
Abstract
The purpose of this research was to investigate the chemical profile, nutritional quality, antioxidant and hypolipidemic effects of Mexican chia seed oil (CSO) in vitro. Chemical characterization of CSO indicated the content of α-linolenic acid (63.64% of total fatty acids) to be the [...] Read more.
The purpose of this research was to investigate the chemical profile, nutritional quality, antioxidant and hypolipidemic effects of Mexican chia seed oil (CSO) in vitro. Chemical characterization of CSO indicated the content of α-linolenic acid (63.64% of total fatty acids) to be the highest, followed by linoleic acid (19.84%), and saturated fatty acid (less than 11%). Trilinolenin content (53.44% of total triacylglycerols (TAGs)) was found to be the highest among seven TAGs in CSO. The antioxidant capacity of CSO, evaluated with ABTS•+ and DPPH methods, showed mild antioxidant capacity when compared with Tocopherol and Catechin. In addition, CSO was found to lower triglyceride (TG) and low-density lipoprotein-cholesterol (LDL-C) levels by 25.8% and 72.9%respectively in a HepG2 lipid accumulation model. As CSO exhibits these chemical and biological characteristics, it is a potential resource of essential fatty acids for human use. Full article
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16 pages, 1643 KiB  
Article
Development of New Analytical Microwave-Assisted Extraction Methods for Bioactive Compounds from Myrtle (Myrtus communis L.)
by Ana V. González de Peredo, Mercedes Vázquez-Espinosa, Estrella Espada-Bellido, Ana Jiménez-Cantizano, Marta Ferreiro-González, Antonio Amores-Arrocha, Miguel Palma, Carmelo G. Barroso and Gerardo F. Barbero
Molecules 2018, 23(11), 2992; https://doi.org/10.3390/molecules23112992 - 16 Nov 2018
Cited by 28 | Viewed by 3629
Abstract
The phenolic compounds and anthocyanins present in myrtle berries are responsible for its beneficial health properties. In the present study, a new, microwave-assisted extraction for the analysis of both phenolic compounds and anthocyanins from myrtle pulp has been developed. Different extraction variables, including [...] Read more.
The phenolic compounds and anthocyanins present in myrtle berries are responsible for its beneficial health properties. In the present study, a new, microwave-assisted extraction for the analysis of both phenolic compounds and anthocyanins from myrtle pulp has been developed. Different extraction variables, including methanol composition, pH, temperature, and sample–solvent ratio were optimized by applying a Box–Behnken design and response surface methodology. Methanol composition and pH were the most influential variables for the total phenolic compounds (58.20% of the solvent in water at pH 2), and methanol composition and temperature for anthocyanins (50.4% of solvent at 50 °C). The methods developed showed high repeatability and intermediate precision (RSD < 5%). Both methods were applied to myrtle berries collected in two different areas of the province of Cadiz (Spain). Hierarchical clustering analysis results show that the concentration of bioactive compounds in myrtle is related to their geographical origin. Full article
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10 pages, 1012 KiB  
Article
Essential Oils from Humulus Lupulus scCO2 Extract by Hydrodistillation and Microwave-Assisted Hydrodistillation
by Katarzyna Tyśkiewicz, Roman Gieysztor, Marcin Konkol, Jan Szałas and Edward Rój
Molecules 2018, 23(11), 2866; https://doi.org/10.3390/molecules23112866 - 03 Nov 2018
Cited by 24 | Viewed by 3799
Abstract
Two different extraction methods were used for a comparative study of essential oils obtained from the Humulus lupulus scCO2 (sc-supercritical) extract: microwave-assisted hydrodistillation (MAHD) and conventional hydrodistillation (HD). As a result, the best conditions for the maximum essential oil production were determined [...] Read more.
Two different extraction methods were used for a comparative study of essential oils obtained from the Humulus lupulus scCO2 (sc-supercritical) extract: microwave-assisted hydrodistillation (MAHD) and conventional hydrodistillation (HD). As a result, the best conditions for the maximum essential oil production were determined for the MAHD method at 335 W microwave power for 30 min at water to raw material ratio of 8:3. The obtained essential oils were enriched in β-myrcene in the amount of 74.13%–89.32% (wt%). Moreover, the first application for determination of the above-mentioned volatile compounds by supercritical fluid chromatography (SFC) with photo-diode array detection (PDA) is presented, which in comparison with gas chromatography coupled with mass spectrometry (GC-MS/MS) resulted in similar values for β-myrcene and α-humulene in obtained samples within less than 1 min. Full article
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14 pages, 1335 KiB  
Article
Simultaneous Identification and Dynamic Analysis of Saccharides during Steam Processing of Rhizomes of Polygonatum cyrtonema by HPLC–QTOF–MS/MS
by Jian Jin, Jia Lao, Rongrong Zhou, Wei He, You Qin, Can Zhong, Jing Xie, Hao Liu, Dan Wan, Shuihan Zhang and Yuhui Qin
Molecules 2018, 23(11), 2855; https://doi.org/10.3390/molecules23112855 - 02 Nov 2018
Cited by 55 | Viewed by 3993
Abstract
The sweet rhizomes of Polygonatum cyrtonema are widely used as a tonic and functional food. A sensitive and rapid analytical method was developed for simultaneous identification and dynamic analysis of saccharides during steam processing in P. cyrtonema using HPLC–QTOF–MS/MS. Fructose, sorbitol, glucose, galactose, [...] Read more.
The sweet rhizomes of Polygonatum cyrtonema are widely used as a tonic and functional food. A sensitive and rapid analytical method was developed for simultaneous identification and dynamic analysis of saccharides during steam processing in P. cyrtonema using HPLC–QTOF–MS/MS. Fructose, sorbitol, glucose, galactose, sucrose, and 1-kestose were identified, as well as a large number of oligosaccharides constituted of fructose units through β-(2→1) or β-(2→6). Polysaccharides and oligosaccharides were decomposed to monosaccharides during a steaming process, since the contents of glucose, galactose, and fructose were increased, while those of sucrose, 1-kestose, and polysaccharides were decreased. The high content of fructose was revealed to be the main determinant for increasing the level of sweetness after steaming. The samples of different repeated steaming times were shown to be well grouped and gradually shift along the PC1 (72.4%) axis by principal component analysis. The small-molecule saccharides, especially fructose, could be considered as markers for the steaming process of rhizomes of P. cyrtonema. Full article
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19 pages, 1856 KiB  
Article
Assessing Nutritional Traits and Phytochemical Composition of Artisan Jams Produced in Comoros Islands: Using Indigenous Fruits with High Health-Impact as an Example of Biodiversity Integration and Food Security in Rural Development
by Dario Donno, Maria Gabriella Mellano, Saandia Hassani, Marta De Biaggi, Isidoro Riondato, Giovanni Gamba, Cristina Giacoma and Gabriele Loris Beccaro
Molecules 2018, 23(10), 2707; https://doi.org/10.3390/molecules23102707 - 20 Oct 2018
Cited by 8 | Viewed by 4153
Abstract
In the Comoros Islands, as in other developing countries, malnutrition and food insecurity affect a very large percentage of the population. Developing fruit-based products in order to make profit, reduce poverty and improve indigenous people diet could be very important for local population [...] Read more.
In the Comoros Islands, as in other developing countries, malnutrition and food insecurity affect a very large percentage of the population. Developing fruit-based products in order to make profit, reduce poverty and improve indigenous people diet could be very important for local population of countries as Comoros Islands. The aim of the present work was to study the chemical composition of jams and jellies produced from seven fruit species harvested in Grand Comore Island. The following parameters were studied sugars and organic acids, total phenolics, total anthocyanins and high-performance liquid chromatography (HPLC) fingerprint of the main phytochemicals. Antioxidant activity was also measured. A multivariate approach (Principal Component Analysis) was performed in order to better characterize the products and to set a potential analytical tool for jam characterisation. Results showed that the analysed products are a good source of polyphenolic constituents, as caffeic and gallic acids, catechin and quercetin and volatile compounds, as limonene and γ-terpinene: these molecules may be considered as suitable markers for these fruit-derived products as characterizing the chromatographic patterns. The characterisation of these products and their nutritional and nutraceutical traits is important as valorisation of local food production for poverty reduction and rural development. Further benefits of this approach include the maintenance of local agro-biodiversity as raw material for fruit-based products and the strengthening of food security practices. Full article
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5 pages, 496 KiB  
Technical Note
Synthesis and Structural Identification of a Biaryl Ether-Linked Zearalenone Dimer
by Julia Keller, Luisa Hantschke, Hajo Haase and Matthias Koch
Molecules 2018, 23(10), 2624; https://doi.org/10.3390/molecules23102624 - 12 Oct 2018
Viewed by 2762
Abstract
A new dimer of the food-relevant mycotoxin zearalenone was isolated after electrochemical and chemical oxidation. The structure was determined as a 16-O-15′-biaryl ether-linked dimer based on spectroscopic analyses (1H- and 13C-NMR, COSY, HMBC, and HSQCAD) and high-resolution mass spectrometry analysis (Q-TOF). Full article
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14 pages, 3193 KiB  
Article
Ultrasensitive Electrochemical Sensor Based on Polyelectrolyte Composite Film Decorated Glassy Carbon Electrode for Detection of Nitrite in Curing Food at Sub-Micromolar Level
by Jingheng Ning, Xin Luo, Min Wang, Jiaojiao Li, Donglin Liu, Hou Rong, Donger Chen and Jianhui Wang
Molecules 2018, 23(10), 2580; https://doi.org/10.3390/molecules23102580 - 09 Oct 2018
Cited by 8 | Viewed by 3568
Abstract
To ensure food quality and safety, developing cost-effective, rapid and precision analytical techniques for quantitative detection of nitrite is highly desirable. Herein, a novel electrochemical sensor based on the sodium cellulose sulfate/poly (dimethyl diallyl ammonium chloride) (NaCS/PDMDAAC) composite film modified glass carbon electrode [...] Read more.
To ensure food quality and safety, developing cost-effective, rapid and precision analytical techniques for quantitative detection of nitrite is highly desirable. Herein, a novel electrochemical sensor based on the sodium cellulose sulfate/poly (dimethyl diallyl ammonium chloride) (NaCS/PDMDAAC) composite film modified glass carbon electrode (NaCS/PDMDAAC/GCE) was proposed toward the detection of nitrite at sub-micromolar level, aiming to make full use of the inherent properties of individual component (biocompatible, low cost, good electrical conductivity for PDMDAAC; non-toxic, abundant raw materials, good film forming ability for NaCS) and synergistic enhancement effect. The NaCS/PDMDAAC/GCE was fabricated by a simple drop-casting method. Electrochemical behaviors of nitrite at NaCS/PDMDAAC/GCE were investigated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). Under optimum conditions, the NaCS/PDMDAAC/GCE exhibits a wide linear response region of 4.0 × 10−8 mol·L−1~1.5 × 10−4 mol·L−1 and a low detection 1imit of 43 nmol·L−1. The NaCS/PDMDAAC shows a synergetic enhancement effect toward the oxidation of nitrite, and the sensing performance is much better than the previous reports. Moreover, the NaCS/PDMDAAC also shows good stability and reproducibility. The NaCS/PDMDAAC/GCE was successfully applied to the determination of nitrite in ham sausage with satisfactory results. Full article
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13 pages, 747 KiB  
Article
The Content of Biogenic Amines in Croatian Wines of Different Geographical Origins
by Ivana Mitar, Ivica Ljubenkov, Nikolina Rohtek, Ante Prkić, Ivana Anđelić and Nenad Vuletić
Molecules 2018, 23(10), 2570; https://doi.org/10.3390/molecules23102570 - 09 Oct 2018
Cited by 19 | Viewed by 3300
Abstract
Samples of white and red wines produced in two different wine-growing regions, coastal (Dalmatia) and continental (Hrvatsko zagorje) of Croatia, were analysed for biogenic amines content. Biogenic amines content was determined, and its concentration levels were associated with the geographical origin of the [...] Read more.
Samples of white and red wines produced in two different wine-growing regions, coastal (Dalmatia) and continental (Hrvatsko zagorje) of Croatia, were analysed for biogenic amines content. Biogenic amines content was determined, and its concentration levels were associated with the geographical origin of the wine. Due to its high sensitivity, HPLC method with ultraviolet detector was used, including the derivatisation step with dansyl chloride. The method was applied to detect and quantify 11 biogenic amines in 48 red and white wines. It was found that both Dalmatian red and white wines are characterised by tryptamine (0.23–1.22 mg L−1), putrescine (0.41–7.5 mg L−1) and ethanolamine (2.87–24.32 mg L−1). White wines from the Hrvatsko zagorje region are characterised by content of isopentylamine (0.31–1.47 mg L−1), putrescine (0.27–1.49 mg L−1) and ethanolamine (3.80–17.96 mg L−1). In contrast to white wines from the Hrvatsko zagorje region, in the red wines, all biogenic amines except ethylamine, were found and equally presented. Full article
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16 pages, 5808 KiB  
Article
Quantification and Confirmation of Fifteen Carbamate Pesticide Residues by Multiple Reaction Monitoring and Enhanced Product Ion Scan Modes via LC-MS/MS QTRAP System
by Ying Zhou, Jian Guan, Weiwei Gao, Shencong Lv and Miaohua Ge
Molecules 2018, 23(10), 2496; https://doi.org/10.3390/molecules23102496 - 29 Sep 2018
Cited by 28 | Viewed by 5351
Abstract
In this research, fifteen carbamate pesticide residues were systematically analyzed by ultra-high performance liquid chromatography–quadrupole-linear ion trap mass spectrometry on a QTRAP 5500 system in both multiple reaction monitoring (MRM) and enhanced product ion (EPI) scan modes. The carbamate pesticide residues were extracted [...] Read more.
In this research, fifteen carbamate pesticide residues were systematically analyzed by ultra-high performance liquid chromatography–quadrupole-linear ion trap mass spectrometry on a QTRAP 5500 system in both multiple reaction monitoring (MRM) and enhanced product ion (EPI) scan modes. The carbamate pesticide residues were extracted from a variety of samples by QuEChERS method and separated by a popular reverse phase column (Waters BEH C18). Except for the current conformation criteria including selected ion pairs, retention time and relative intensities from MRM scan mode, the presence of carbamate pesticide residues in diverse samples, especially some doubtful cases, could also be confirmed by the matching of carbamate pesticide spectra via EPI scan mode. Moreover, the fragmentation routes of fifteen carbamates were firstly explained based on the mass spectra obtained by a QTRAP system; the characteristic fragment ion from a neutral loss of CH3NCO (−57 Da) could be observed. The limits of detection and quantification for fifteen carbamates were 0.2–2.0 μg kg−1 and 0.5–5.0 μg kg−1, respectively. For the intra- (n = 3) and inter-day (n = 15) precisions, the recoveries of fifteen carbamates from spiked samples ranged from 88.1% to 118.4%, and the coefficients of variation (CVs) were all below 10%. The method was applied to pesticide residues detection in fruit, vegetable and green tea samples taken from local markets, in which carbamates were extensively detected but all below the standard of maximum residue limit. Full article
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15 pages, 3027 KiB  
Article
Selection and Identification of Novel Aptamers Specific for Clenbuterol Based on ssDNA Library Immobilized SELEX and Gold Nanoparticles Biosensor
by Xixia Liu, Qi Lu, Sirui Chen, Fang Wang, Jianjun Hou, Zhenlin Xu, Chen Meng, Tianyuan Hu and Yaoyao Hou
Molecules 2018, 23(9), 2337; https://doi.org/10.3390/molecules23092337 - 13 Sep 2018
Cited by 25 | Viewed by 4617
Abstract
We describe a multiple combined strategy to discover novel aptamers specific for clenbuterol (CBL). An immobilized ssDNA library was used for the selection of specific aptamers using the systematic evolution of ligands by exponential enrichment (SELEX). Progress was monitored using real-time quantitative PCR [...] Read more.
We describe a multiple combined strategy to discover novel aptamers specific for clenbuterol (CBL). An immobilized ssDNA library was used for the selection of specific aptamers using the systematic evolution of ligands by exponential enrichment (SELEX). Progress was monitored using real-time quantitative PCR (Q-PCR), and the enriched library was sequenced by high-throughput sequencing. Candidate aptamers were picked and preliminarily identified using a gold nanoparticles (AuNPs) biosensor. Bioactive aptamers were characterized for affinity, circular dichroism (CD), specificity and sensitivity. The Q-PCR amplification curve increased and the retention rate was about 1% at the eighth round. Use of the AuNPs biosensor and CD analyses determined that six aptamers had binding activity. Affinity analysis showed that aptamer 47 had the highest affinity (Kd = 42.17 ± 8.98 nM) with no cross reactivity to CBL analogs. Indirect competitive enzyme linked aptamer assay (IC-ELAA) based on a 5′-biotin aptamer 47 indicated the limit of detection (LOD) was 0.18 ± 0.02 ng/L (n = 3), and it was used to detect pork samples with a mean recovery of 83.33–97.03%. This is the first report of a universal strategy including library fixation, Q-PCR monitoring, high-throughput sequencing, and AuNPs biosensor identification to select aptamers specific for small molecules. Full article
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15 pages, 3619 KiB  
Article
Novel Electrochemical Sensors Based on Cuprous Oxide-Electrochemically Reduced Graphene Oxide Nanocomposites Modified Electrode toward Sensitive Detection of Sunset Yellow
by Quanguo He, Jun Liu, Xiaopeng Liu, Yonghui Xia, Guangli Li, Peihong Deng and Dongchu Chen
Molecules 2018, 23(9), 2130; https://doi.org/10.3390/molecules23092130 - 24 Aug 2018
Cited by 51 | Viewed by 4332
Abstract
Control and detection of sunset yellow is an utmost demanding issue, due to the presence of potential risks for human health if excessively consumed or added. Herein, cuprous oxide-electrochemically reduced graphene nanocomposite modified glassy carbon electrode (Cu2O-ErGO/GCE) was developed for the [...] Read more.
Control and detection of sunset yellow is an utmost demanding issue, due to the presence of potential risks for human health if excessively consumed or added. Herein, cuprous oxide-electrochemically reduced graphene nanocomposite modified glassy carbon electrode (Cu2O-ErGO/GCE) was developed for the determination of sunset yellow. The Cu2O-ErGO/GCE was fabricated by drop-casting Cu2O-GO dispersion on the GCE surface following a potentiostatic reduction of graphene oxide (GO). Scanning electron microscope and X-ray powder diffractometer was used to characterize the morphology and microstructure of the modification materials, such as Cu2O nanoparticles and Cu2O-ErGO nanocomposites. The electrochemical behavior of sunset yellow on the bare GCE, ErGO/GCE, and Cu2O-ErGO/GCE were investigated by cyclic voltammetry and second-derivative linear sweep voltammetry, respectively. The analytical parameters (including pH value, sweep rate, and accumulation parameters) were explored systematically. The results show that the anodic peak currents of Cu2O-ErGO /GCE are 25-fold higher than that of the bare GCE, due to the synergistic enhancement effect between Cu2O nanoparticles and ErGO sheets. Under the optimum detection conditions, the anodic peak currents are well linear to the concentrations of sunset yellow, ranging from 2.0 × 10−8 mol/L to 2.0 × 10−5 mol/L and from 2.0 × 10−5 mol/L to 1.0 × 10−4 mol/L with a low limit of detection (S/N = 3, 6.0 × 10−9 mol/L). Moreover, Cu2O-ErGO/GCE was successfully used for the determination of sunset yellow in beverages and food with good recovery. This proposed Cu2O-ErGO/GCE has an attractive prospect applications on the determination of sunset yellow in diverse real samples. Full article
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