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Methods in Food Analysis

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A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Analytical Chemistry".

Deadline for manuscript submissions: closed (30 April 2022) | Viewed by 21297

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Prof. Dr. Clinio Locatelli

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Department of Chemistry “Giacomo Ciamician”, Alma Mater Studiorum University of Bologna, Via Selmi 2, I-40126 Bologna, Italy
Interests: analytical methods set up; environmental field; food contaminants; spectroscopy; voltammetry
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Prof. Dr. Dora Melucci

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Department of Chemistry “Giacomo Ciamician”, Alma Mater Studiorum University of Bologna, Via Selmi 2, I-40126 Bologna, Italy
Interests: chemometrics; environmental chemistry; forensics; food chemistry; pharmaceutics
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Dr. Marcello Locatelli

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Department of Pharmacy, University “G. d\'Annunzio” of Chieti and Pescara, Chieti, Italy
Interests: innovative (micro)extraction procedures; hyphenated instrument configurations; bioactive compounds; characterization; fingerprints; method validation; HPLC; mass spectrometry; biological matrices; chromatography; analytical chemistry; sample preparation; green analytical methodologies
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Special Issue Information

Dear Colleagues,

Nowadays the possibility of analysing, tracing, and certifying food products (as well as supplements) is of fundamental importance in order to guarantee not only the quality of the product, but above all to safeguard the health of the consumer.

In this perspective, the availability of analytical procedures, instrumental configurations, and statistical and chemometric methods that can be integrated to maximize analytical information is fundamental.

An element not to be overlooked is also the scalability of the processes from the laboratory to the industrial level and the quality control and traceability (as well as the verification of the authenticity of the product).

This Special Issue will highlight and describe the latest improvements in instrument configurations, techniques developed, and particularly, innovative statistical approaches applied to analyse the data. Additionally, it aims to attract contributions on all aspects linked to the different approaches used for food analysis, focusing particularly on the fundamental parameters of interest to set-up an analytical procedure, such as precision and trueness (that together give accuracy); the limits of detection and quantification; selectivity; and, especially, sensitivity, GAC (green analytical chemistry) approach, quality control and traceability

Prof. Dr. Clinio Locatelli
Prof. Dr. Dora Melucci
Prof. Dr. Marcello Locatelli
Guest Editors

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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

Food analysis
Food additives analysis
Adulteration/sophistication
Quality control
Method development and validation
Chemometrics

Published Papers (9 papers)

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Research

13 pages, 1111 KiB

Open AccessArticle

Determination of Free Amino Acids in Milk, Colostrum and Plasma of Swine via Liquid Chromatography with Fluorescence and UV Detection

by Roberto Gotti, Erika Esposito, Diana Luise, Stefano Tullio, Nicolò Interino, Paolo Trevisi and Jessica Fiori

Molecules 2022, 27(13), 4153; https://doi.org/10.3390/molecules27134153 - 28 Jun 2022

Cited by 4 | Viewed by 2416

Abstract

Amino acids are ubiquitous components of mammalian milk and greatly contribute to its nutritional value. The compositional analysis of free amino acids is poorly reported in the literature even though their determination in the biological fluids of livestock animals is necessary to establish possible nutritional interventions. In the present study, the free amino acid profiles in mature swine milk, colostrum and plasma were assessed using a targeted metabolomics approach. In particular, 20 amino acids were identified and quantified via two alternative and complementary reversed-phase HPLC methods, involving two stationary phases based on core-shell technology, i.e., Kinetex C18 and Kinetex F5, and two detection systems, i.e., a diode array detector (DAD) and a fluorescence detector (FLD). The sample preparation involved a de-proteinization step, followed by pre-chromatographic derivatization with 9-fluorenylmethylchloroformate (FMOC-Cl). The two optimized methods were validated for specificity, linearity, sensitivity, matrix effect, accuracy and precision and the analytical performances were compared. The analytical methods proved to be suitable for free amino acid profiling in different matrices with high sensitivity and specificity. The correlations among amino acid levels in different biological fluids can be useful for the evaluation of physio-pathological status and to monitor the effects of therapeutic or nutritional interventions in humans and animals. Full article

(This article belongs to the Special Issue Methods in Food Analysis)

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21 pages, 3005 KiB

Open AccessArticle

Detection, Identification and Size Distribution of Silver Nanoparticles (AgNPs) in Milk and Migration Study for Breast Milk Storage Bags

by Bin Li, Sew Lay Chua, Dingyi Yu, Sheot Harn Chan and Angela Li

Molecules 2022, 27(8), 2539; https://doi.org/10.3390/molecules27082539 - 14 Apr 2022

Cited by 6 | Viewed by 1949

Abstract

The engineered silver nanoparticles (AgNPs) have been widely used in various food contact materials (FCMs) based on their antibacterial properties. This widespread use of nanosilver has, however, increased the risk of exposure of AgNPs to human due to their migration from FCMs causing a potential hazard present in foods. Therefore, it is important to establish a reliable and practical method for the detection of AgNPs in food matrices to support risk assessment on AgNPs exposure. Taking the examples of milk and AgNPs-containing breast milk storage bags, this study established an approach for size characterization and quantification of AgNPs in milk and evaluated the relevant silver migration, based on enzymatic digestion and the analysis by asymmetric flow field–flow fractionation (AF4) hyphenated with inductively coupled plasma mass spectrometry (ICP-MS) and single particle inductively coupled plasma mass spectrometry (SP-ICP-MS). No migration of AgNPs was found from breast milk storage bags under various simulated storage conditions as well as extreme scenarios. The suitability and reliability of this method were also validated by the determination of multiple parameters, including accuracy, repeatability, limit of detection (LOD), limit of quantification (LOQ), and recovery, for AF4-ICP-MS and SP-ICP-MS, respectively, with good and overall acceptable evaluation results obtained for all. The established and validated approach was demonstrated to be suitable for the characterization and quantitation of AgNPs in milk as well as the analysis of their migration from breast milk storage bags. Full article

(This article belongs to the Special Issue Methods in Food Analysis)

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18 pages, 1675 KiB

Open AccessArticle

Analysis of Biogenic Amines Using Immunoassays, HPLC, and a Newly Developed IC-MS/MS Technique in Fish Products—A Comparative Study

by Drago Kočar, Sevim Köse, Serkan Koral, Bekir Tufan, Andrej Ščavničar and Matevž Pompe

Molecules 2021, 26(20), 6156; https://doi.org/10.3390/molecules26206156 - 12 Oct 2021

Cited by 11 | Viewed by 2123

Abstract

In this study, comparative analyses were carried out with ion chromatography mass-spectrometry (IC-MS/MS) which has no derivatization step, high-performance liquid chromatography (HPLC) technique, as well as two quantitative and two semi-quantitative immunoassays. The results demonstrated that HPLC and quantitative immunoassay methods were well-correlated with IC-MS/MS in determining histamine in various types of fish products. The best correlation was observed with the HistaSure ELISA Fast Track kit (R² = 0.9903). More than half of the values (68%) obtained by two methods were also statistically similar. The results of semi-quantitative test kits also supported histamine values estimated by quantitative methods, with some exceptions. The best results were found for HistaSure Lateral Flow in supporting the quantitative techniques. Therefore, these methods are found suitable for monitoring histamine in fish products in terms of food safety. Good correlations were also observed HPLC and IC-MS/MS in determining cadaverine, putrescine, and tyramine with the highest value observed for tyramine as R² = 0.9785. However, no correlation was observed for other biogenic amines, and the majority of the results were significantly different from each other for these amines (p < 0.05). The differences may be caused by the drawbacks reported previously for HPLC. However, further studies are required to confirm the possible effects. This study provides a comparative evaluation of several methods in terms of their suitability in determining biogenic amines in fish products for both monitoring and regulatory purposes. Full article

(This article belongs to the Special Issue Methods in Food Analysis)

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16 pages, 799 KiB

Open AccessArticle

Benefits and Pitfalls of HPLC Coupled to Diode-Array, Charged Aerosol, and Coulometric Detections: Effect of Detection on Screening of Bioactive Compounds in Apples

by Marcela Hollá, Aneta Bílková, Pavel Jakubec, Stanislava Košková, Hana Kočová Vlčková, Dalibor Šatínský, František Švec and Hana Sklenářová

Molecules 2021, 26(11), 3246; https://doi.org/10.3390/molecules26113246 - 28 May 2021

Cited by 5 | Viewed by 2811

Abstract

The new screening method for rapid evaluation of major phenolic compounds in apples has been developed. Suitability of coupling HPLC/UHPLC separation with the diode-array detection and universal charged aerosol detection with respect to the presence of interfering substances was tested. Characteristics of both detection techniques were compared and method linearity, limits of detection and quantitation, and selectivity of them determined. Student t-test based on slopes of calibration plots was applied for the detailed comparison. The diode-array detection provided the best results regarding sensitivity and selectivity of the developed method in terms of evaluation of phenolics profiles. The response of the charged aerosol detector was negatively affected by co-eluting substances during rapid-screening analyses. Coulometric detection was used for advanced characterization of extracts in terms of antioxidant content and strength to obtain more complex information concerning sample composition. This detection also allowed evaluation of unidentified compounds with antioxidant activity. HPLC/UHPLC separation using a combination of diode-array and coulometric detectors thus represented the best approach enabling quick, yet complex characterization of bioactive compounds in apples. Full article

(This article belongs to the Special Issue Methods in Food Analysis)

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9 pages, 1433 KiB

Open AccessArticle

Non-Invasive Identification of Nutrient Components in Grain

by Charles Farber, A. S. M. Faridul Islam, Endang M. Septiningsih, Michael J. Thomson and Dmitry Kurouski

Molecules 2021, 26(11), 3124; https://doi.org/10.3390/molecules26113124 - 24 May 2021

Cited by 6 | Viewed by 1780

Abstract

Digital farming is a modern agricultural concept that aims to maximize the crop yield while simultaneously minimizing the environmental impact of farming. Successful implementation of digital farming requires development of sensors to detect and identify diseases and abiotic stresses in plants, as well as to probe the nutrient content of seeds and identify plant varieties. Experimental evidence of the suitability of Raman spectroscopy (RS) for confirmatory diagnostics of plant diseases was previously provided by our team and other research groups. In this study, we investigate the potential use of RS as a label-free, non-invasive and non-destructive analytical technique for the fast and accurate identification of nutrient components in the grains from 15 different rice genotypes. We demonstrate that spectroscopic analysis of intact rice seeds provides the accurate rice variety identification in ~86% of samples. These results suggest that RS can be used for fully automated, fast and accurate identification of seeds nutrient components. Full article

(This article belongs to the Special Issue Methods in Food Analysis)

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17 pages, 1647 KiB

Open AccessArticle

Inorganic Elements in Mytilus galloprovincialis Shells: Geographic Traceability by Multivariate Analysis of ICP-MS Data

by Tiziana Forleo, Alessandro Zappi, Dora Melucci, Martina Ciriaci, Francesco Griffoni, Simone Bacchiocchi, Melania Siracusa, Tamara Tavoloni and Arianna Piersanti

Molecules 2021, 26(9), 2634; https://doi.org/10.3390/molecules26092634 - 30 Apr 2021

Cited by 9 | Viewed by 1797

Abstract

The international seafood trade is based on food safety, quality, sustainability, and traceability. Mussels are bio-accumulative sessile organisms that need regular control to guarantee their safe consumption. However, no well-established and validated methods exist to trace mussel origin, even if several attempts have been made over the years. Recently, an inorganic multi-elemental fingerprint coupled to multivariate statistics has increasingly been applied in food quality control. The mussel shell can be an excellent reservoir of foreign inorganic chemical species, allowing recording long-term environmental changes. The present work investigates the multi-elemental composition of mussel shells, including Al, Cu, Cr, Zn, Mn, Cd, Co, U, Ba, Ni, Pb, Mg, Sr, and Ca, determined by inductively-coupled plasma mass-spectrometry in Mytilus galloprovincialis collected along the Central Adriatic Coast (Marche Region, Italy) at 25 different sampling sites (18 farms and 7 natural banks) located in seven areas. The experimental data, coupled with chemometric approaches (principal components analysis and linear discriminant analysis), were used to create a statistical model able to discriminate samples as a function of their production site. The LDA model is suitable for achieving a correct assignment of >90% of individuals sampled to their respective harvesting locations and for being applied to counteract fraud. Full article

(This article belongs to the Special Issue Methods in Food Analysis)

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16 pages, 1656 KiB

Open AccessArticle

Identification of Selected Tuna Species in Commercial Products

by Eliska Servusova and Zora Piskata

Molecules 2021, 26(4), 1137; https://doi.org/10.3390/molecules26041137 - 20 Feb 2021

Cited by 10 | Viewed by 2354

Abstract

This study was conducted to develop systems for the identification of four tuna species (skipjack tuna Katsuwonus pelamis, yellowfin tuna Thunnus albacares, bullet tuna Auxis sp. and Atlantic bonito Sarda sp). At first, raw samples of these species and a mix intended as internal control were prepared for the authentication of fish muscle tissue of the genus Thunnus sp., Auxis sp. and Sarda sp. DNA from raw muscle tissue, the mix and samples was extracted with the DNeasy mericon Food Kit (Qiagen GmbH, Hilden, Germany). The concentration and purity of DNA in raw samples were evaluated using a spectrophotometer. Primers and probe sequences were specifically designed to identify the selected species. In addition, primers and a probe for the endogenous 12S rRNA gene were designed to determine the presence of amplifiable fish (especially tuna) DNA in samples. Furthermore, the species specificity of the designed primers and probes was verified in DNA samples of various tuna and bonito species. Limit of detection for the selected species was calculated as well as the coefficient of determination R² and efficiency of real-time PCR testing was determined. To evaluate the developed real-time PCR methods, 70 commercial tuna products were analysed. The results show that mislabelling of fish products can still be encountered and, moreover, the presence of an additional species can be identified. Full article

(This article belongs to the Special Issue Methods in Food Analysis)

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13 pages, 552 KiB

Open AccessArticle

A Dilute and Shoot Strategy for Determining Alternaria Toxins in Tomato-Based Samples and in Different Flours Using LC-IDMS Separation

by Ádám Tölgyesi, Tamás Farkas, Mária Bálint, Thomas J. McDonald and Virender K. Sharma

Molecules 2021, 26(4), 1017; https://doi.org/10.3390/molecules26041017 - 15 Feb 2021

Cited by 7 | Viewed by 2109

Abstract

Alternaria toxins are emerging mycotoxins whose regulation and standardization are in progress by the European Commission and the European Committee for Standardization. This paper describes a dilute and shoot approach to determine five Alternaria toxins in selected food samples using liquid chromatography–tandem mass spectrometry (LC-MS/MS). The strategy involves sample extraction with acidified aqueous methanol, followed by a solvent change accomplished via sample evaporation and reconstitution. The quantification is based on isotope dilution, applying all corresponding isotopically labeled internal standards to compensate possible matrix effects of the analysis. The main advantages of the present method over other existing methods includes simple and effective sample preparation, as well as detection with high sensitivity. The five-fold sample dilution can decrease matrix effects, which were evaluated with both external and internal standard methods. The results demonstrated a limit of quantification lower than 1.0 µg/kg for all five analytes for the first time. The newly presented method showed acceptable accuracy (52.7–111%) when analyzing naturally contaminated and spiked standard samples at the described levels. The method was validated for tomato-based and flour samples (wheat, rye, and maize). The absolute recovery ranged from 66.7% to 91.6% (RSD < 10%). The developed method could be an alternative approach for those laboratories that exclude sample cleanup and pre-concentration of state-of-the-art instruments with enhanced sensitivity. Full article

(This article belongs to the Special Issue Methods in Food Analysis)

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13 pages, 2883 KiB

Open AccessArticle

A QuEChERS-HPLC-MS/MS Method with Matrix Matching Calibration Strategy for Determination of Imidacloprid and Its Metabolites in Procambarus clarkii (Crayfish) Tissues

by Qiuhong Yang, Xiaohui Ai, Jing Dong, Yongtao Liu, Shun Zhou, Yibin Yang and Ning Xu

Molecules 2021, 26(2), 274; https://doi.org/10.3390/molecules26020274 - 07 Jan 2021

Cited by 7 | Viewed by 2585

Abstract

We developed a method for determination of imidacloprid and its metabolites 5-hydroxy imidacloprid, olefin imidacloprid, imidacloprid urea and 6-chloronicotinic acid in Procambarus clarkii (crayfish) tissues using quick, easy, cheap, effective, rugged, and safe (QuEChERS) and high-performance liquid chromatography-triple quadrupole mass spectrometry. Samples (plasma, cephalothorax, hepatopancrea, gill, intestine, and muscle) were extracted with acetonitrile containing 0.1% acetic acid and cleaned up using a neutral alumina column containing a primary secondary amine. The prepared samples were separated using reverse phase chromatography and scanned in the positive and negative ion multiple reaction-monitoring modes. Under the optimum experimental conditions, spiked recoveries for these compounds in P. clarkii samples ranged from 80.6 to 112.7% with relative standard deviations of 4.2 to 12.6%. The limits of detection were 0.02–0.5 μg·L⁻¹, the limits of quantification were 0.05–2.0 μg·L⁻¹ and the method of quantification was 0.05–2.0 μg·kg⁻¹. The method is rapid, simple, sensitive and suitable for rapid determination and analysis of imidacloprid and its metabolites in P. clarkii tissues. Full article

(This article belongs to the Special Issue Methods in Food Analysis)

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