Identification, Characterization and Quantification of Food Compounds Using Chromatography and Mass Spectrometry

A special issue of Foods (ISSN 2304-8158). This special issue belongs to the section "Food Analytical Methods".

Deadline for manuscript submissions: 10 June 2024 | Viewed by 38791

Special Issue Editors


E-Mail Website1 Website2
Guest Editor
Department of Pharmaceutical Sciences and Medicines (DCFM), Faculty of Pharmacy, University of Lisbon, Avenida Prof. Gama Pinto, 1649-019 Lisbon, Portugal
Interests: mass spectrometry; high-performance liquid chromatography; gas chromatography; chromatographic method development; phenolic compounds; food bioactive compounds; food security
iMed.ULisboa—Research Institute for Medicines, Faculty of Pharmacy, University of Lisbon, Avenida Prof. Gama Pinto, 1649-019 Lisbon, Portugal
Interests: natural products; bioactive compounds; terpenes; phenolics; plant derived compounds; medicinal plants; natural products chemistry; mass spectrometry; multidrug resistance; medicinal chemistry
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Special Issue Information

Dear Colleagues,

Chromatography has become indispensable for the qualitative and quantitative analysis of a vast number of compounds in complex mixtures. In particular, gas chromatography (GC) and high-performance liquid chromatography (HPLC) have been widely used in different fields of food science. These techniques are often coupled to mass spectrometers, which are increasingly recognised as powerful tools for the unequivocal identification of specific compounds. HPLC-MS and GC-MS have been subjected to extensive and continuous improvements, allowing for the detection of bioactive compounds, food contaminants, toxins and aroma compounds, in different food matrices. Notwithstanding the importance of technological improvements, the development of new methods of extraction has made a remarkable contribution to food analysis.

In recent years, there has been a growing interest in the analysis of trace levels of several compounds, which may have a relevant impact on food quality. Despite the recent advances, the analysis of components at very low levels in complex matrices is still often a challenge. Therefore, this Special Issue in Foods aims to gather the latest research and advancements addressing the application of chromatographic and mass spectrometry methods in food science.

We encourage authors to share their scientific achievements in original research or review articles regarding the applications of these techniques in the analysis of naturally occurring compounds, food additives and contaminants, in different food sources. Potential topics include, but are not limited to, the identification and quantitation of food bioactive compounds, flavor and aroma compounds, environmental pollutants, adulterants, pesticides, mycotoxins, natural toxins, veterinary and human drugs, toxins generated during food processing and packaging materials. The development and validation of extraction and chromatographic methods, the identification of existing challenges and possible future approaches will also be considered.

We look forward to your valued contribution.

Dr. Andreia Bento Silva
Dr. Noelia Duarte
Guest Editors

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Keywords

  • food analysis
  • food security
  • food authenticity
  • natural products
  • aroma compounds
  • bioactive compounds
  • liquid chromatography
  • gas chromatography
  • mass spectrometry
  • chromatographic method development
  • sample preparation

Published Papers (9 papers)

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Research

12 pages, 2616 KiB  
Article
Exploration and Improvement of Acid Hydrolysis Conditions for Inulin-Type Fructans Monosaccharide Composition Analysis: Monosaccharide Recovery and By-Product Identification
by Xinyan Zong, Ningyu Lei, Junyi Yin, Weiwei He, Shaoping Nie and Mingyong Xie
Foods 2024, 13(8), 1241; https://doi.org/10.3390/foods13081241 - 18 Apr 2024
Viewed by 551
Abstract
Acid hydrolysis serves as the primary method for determining the monosaccharide composition of polysaccharides. However, inappropriate acid hydrolysis conditions may catalyze the breakdown of monosaccharides such as fructans (Fru), generating non-sugar by-products that affect the accuracy of monosaccharide composition analysis. In this study, [...] Read more.
Acid hydrolysis serves as the primary method for determining the monosaccharide composition of polysaccharides. However, inappropriate acid hydrolysis conditions may catalyze the breakdown of monosaccharides such as fructans (Fru), generating non-sugar by-products that affect the accuracy of monosaccharide composition analysis. In this study, we determined the monosaccharide recovery rate and non-sugar by-product formation of inulin-type fructan (ITF) and Fru under varied acid hydrolysis conditions using HPAEC-PAD and UPLC-Triple-TOF/MS, respectively. The results revealed significant variations in the recovery rate of Fru within ITF under different hydrolysis conditions, while glucose remained relatively stable. Optimal hydrolysis conditions for achieving a relatively high monosaccharide recovery rate for ITF entailed 80 °C, 2 h, and 1 M sulfuric acid. Furthermore, we validated the stability of Fru during acid hydrolysis. The results indicated that Fru experienced significant degradation with an increasing temperature and acid concentration, with a pronounced decrease observed when the temperature exceeds 100 °C or the H2SO4 concentration surpasses 2 M. Finally, three common by-products associated with Fru degradation, namely 5-hydroxymethyl-2-furaldehyde, 5-methyl-2-furaldehyde, and furfural, were identified in both Fru and ITF hydrolysis processes. These findings revealed that the degradation of Fru under acidic conditions was a vital factor leading to inaccuracies in determining the Fru content during ITF monosaccharide analysis. Full article
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16 pages, 2435 KiB  
Article
A Culinary and Medicinal Gem: Exploring the Phytochemical and Functional Properties of Thai Basil
by Panita Prasongdee, Kakanang Posridee, Anant Oonsivilai and Ratchadaporn Oonsivilai
Foods 2024, 13(4), 632; https://doi.org/10.3390/foods13040632 - 19 Feb 2024
Cited by 1 | Viewed by 701
Abstract
This study aimed to comprehensively evaluate the potential health benefits of Thai basil extracts from two species, Ocimum basilicum var. thyrsiflorum and Ocimum basilicum cv. Jumbo 4320, by investigating their bioactivities, phytochemical composition, and in vitro antioxidant, antimicrobial, and antithrombotic activities. Thai basil [...] Read more.
This study aimed to comprehensively evaluate the potential health benefits of Thai basil extracts from two species, Ocimum basilicum var. thyrsiflorum and Ocimum basilicum cv. Jumbo 4320, by investigating their bioactivities, phytochemical composition, and in vitro antioxidant, antimicrobial, and antithrombotic activities. Thai basil extracts from two species (Ocimum basilicum var. thyrsiflorum and cv. Jumbo 4320) were obtained using water, ethanol, and ethyl acetate. Phytochemical analysis revealed chlorophylls, carotenoids, and diverse phenolic compounds. Its water extract boasted the highest total phenolics (459.62 ± 3.07 mg GAE/100 g), outperforming ethanol and ethyl acetate extracts (171.20 ± 1.10 and 66.02 ± 0.99 mg GAE/100 g, respectively). The ethanol extract of Jumbo 4320 also reigned supreme in total flavonoids (557.12 ± 14.27 mg CE/100 g), surpassing its counterparts (209.07 ± 23.31 and 131.41 ± 0.37 mg CE/100 g). O. basilicum cv. Jumbo 4320 extracts exhibited superior antioxidant activity by various assays. Jumbo 4320′s water extract further dominated in the DPPH assay (IC50 48.52 ± 1.15 mg/mL), demonstrating superior free radical scavenging compared to ethanol and ethyl acetate extracts (IC50 60.54 ± 0.52 and 82.09 ± 3.18 mg/mL), respectively. While thyrsiflorum’s ethanol extract claimed the top spot in the FRAP assay (0.0186 ± 0.00 mmol Fe2+/g), Jumbo 4320′s water extract showcased the highest cellular antioxidant activity (80.62 ± 0.00% relative fluorescence intensity) in the DCFH-DA assay. Interestingly, Ocimum basilicum var. thyrsiflorum extracts demonstrated stronger antithrombotic activity at prolonging the prothrombin time at 78.3 ± 17.56 s. While the antimicrobial activity against most tested pathogens was limited, both species’ extracts inhibited Bacillus cereus. These findings suggest the potential of Thai basil extracts, particularly from Jumbo 4320, as functional food ingredients with antioxidant and antithrombotic properties. Full article
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13 pages, 738 KiB  
Article
A Suitable HPLC-MS/MS Methodology for the Detection of Oxytetracycline, Enrofloxacin, and Sulfachloropyridazine Residues in Lettuce Plants
by Karina Yévenes, María José Ibáñez, Ekaterina Pokrant, Andrés Flores, Matías Maturana, Aldo Maddaleno and Javiera Cornejo
Foods 2024, 13(1), 153; https://doi.org/10.3390/foods13010153 - 2 Jan 2024
Viewed by 1196
Abstract
Oxytetracycline (OTC), enrofloxacin (EFX), and sulfachloropyridazine (SCP) are critically important antimicrobials (AMs) in both human and veterinary medicine, where they are widely used in farm animals. Lettuce has become a matrix of choice for studying the presence of residues of these AMs in [...] Read more.
Oxytetracycline (OTC), enrofloxacin (EFX), and sulfachloropyridazine (SCP) are critically important antimicrobials (AMs) in both human and veterinary medicine, where they are widely used in farm animals. Lettuce has become a matrix of choice for studying the presence of residues of these AMs in plants, as the concentrations of residues detected in lettuce can range from ng to mg. While several analytical methodologies have been developed for the purpose of detecting AMs in lettuce, these currently do not detect both the parent compound and its active metabolites or epimers, such as in the case of ciprofloxacin (CFX) and 4-epi-oxitetracycline (4-epi-OTC), which also pose a risk to public health and the environment due to their AM activity. In light of this situation, this work proposes an analytical method that was developed specifically to allow for the detection of OTC, 4-epi-OTC, EFX, CFX, and SCP in a lettuce matrix. This method uses acetonitrile, methanol, 0.5% formic acid, and McIlvaine-EDTA buffer as extraction solvents, and dispersive solid-phase extraction (dSPE) for the clean-up. The analytes were detected using a liquid chromatography technique coupled to mass spectrometry (HPLC-MS/MS). Parameters such as the specificity, linearity, recovery, precision, limit of detection, and limit (LOD) of quantification (LOQ) were calculated according to the recommendations established in the European Union decision 2021/808/EC and VICH GL2: Validation of analytical procedures. The LOQ for the analytes OTC, 4-epi-OTC, CFX, and SCP was 1 μg·kg−1, whereas for EFX, it was 5 μg·kg−1 dry weight. All calibration curves showed a coefficient of determination (R2) of >0.99. The recovery levels ranged from 93.0 to 110.5% and the precision met the acceptance criteria, with a coefficient of variation of ≤14.02%. Therefore, this methodology allows for the precise and reliable detection and quantification of these analytes. The analysis of commercial samples confirmed the suitability of this method. Full article
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17 pages, 1485 KiB  
Article
Matrix Effect Evaluation in GC/MS-MS Analysis of Multiple Pesticide Residues in Selected Food Matrices
by Mateja Bulaić Nevistić and Marija Kovač Tomas
Foods 2023, 12(21), 3991; https://doi.org/10.3390/foods12213991 - 31 Oct 2023
Cited by 1 | Viewed by 1238
Abstract
Multi-analyte methods based on QuEChERS sample preparation and chromatography/mass spectrometry determination are indispensable in monitoring pesticide residues in the feed and food chain. QuEChERS method, even though perceived as convenient and generic, can contribute to sample matrix constituents’ introduction to the measuring system [...] Read more.
Multi-analyte methods based on QuEChERS sample preparation and chromatography/mass spectrometry determination are indispensable in monitoring pesticide residues in the feed and food chain. QuEChERS method, even though perceived as convenient and generic, can contribute to sample matrix constituents’ introduction to the measuring system and possibly affect analytical results. In this study, matrix effects (ME) were investigated in four food matrices of plant origin (apples, grapes, spelt kernels, and sunflower seeds) during GC-MS/MS analysis of >200 pesticide residues using QuEChERS sample preparation. Data analysis revealed considerable analyte signal enhancement and suppression: strong enhancement was observed for the majority of analytes in two matrices within the commodity groups with high water content—apples, and high acid and water content—grapes (73.9% MES and 72.5% MEA, and 77.7% MES and 74.9% MEA, respectively), while strong suppression was observed for matrices within the commodity groups with high starch/protein content and low water and fat content—spelt kernels, and high oil content and very low water content—sunflower seeds (82.1% MES and 82.6% MEA, and 65.2% MES and 70.0% MEA, respectively). Although strong matrix effects were the most common for all investigated matrices, the use of matrix-matched calibration for each sample type enabled satisfactory method performance, i.e., recoveries for the majority of analytes (up to roughly 90%, depending on the fortification level and matrix type), which was also externally confirmed through participation in proficiency testing schemes for relevant food commodity groups with the achieved z-scores within acceptable range ≤ |2|. Full article
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14 pages, 1519 KiB  
Article
Geographical Indication Characteristics of Aroma and Phenolic Acids of the Changping Strawberry
by Linxia Wu, Xinlu Wang, Jianqiang Hao, Ning Zhu and Meng Wang
Foods 2023, 12(21), 3889; https://doi.org/10.3390/foods12213889 - 24 Oct 2023
Cited by 1 | Viewed by 948
Abstract
Strawberry is the most consumed berry fruit worldwide due to its unique aroma and high nutritive value. This fruit is also an important source of phenolic compounds. Changping strawberries are recognized as a national agricultural product of geographical indication (GI) due to their [...] Read more.
Strawberry is the most consumed berry fruit worldwide due to its unique aroma and high nutritive value. This fruit is also an important source of phenolic compounds. Changping strawberries are recognized as a national agricultural product of geographical indication (GI) due to their unique flavor. Widely accepted standards for identifying GI strawberries from non-GI strawberries are currently unavailable. This study compared the aroma and phenolic acid composition of GI and non-GI strawberries. Furthermore, the characteristic aroma and phenolic acid markers of GI strawberries were determined. A classification model based on the markers was established using Fisher discriminant analysis (FDA). In this study, six groups of strawberries with variety name of “Hongyan”, including GI strawberries from Changping and non-GI strawberries from Changping, Miyun, Pinggu, Shunyi, and Tongzhou, were collected. A total of 147 volatile substances were discovered using gas chromatography–tandem mass spectrometry. The contents of a few compounds principally responsible for the distinctive aroma in GI strawberries were in the top three of the six groups, providing GI strawberries with a generally pleasant fragrance. OPLS–DA identified isoamyl butyrate and trans-2-octen-1-ol as characteristic markers. Enrichment analysis indicated that beta-oxidation of very long-chain fatty acids, mitochondrial beta-oxidation of very long-chain fatty acids, fatty acid biosynthesis, and butyrate metabolism played critical roles in volatile compound biosynthesis. The total phenolic content was 24.41–36.46 mg/kg of fresh weight. OPLS–DA results revealed that cinnamic acid could be used as a characteristic phenolic acid marker of GI strawberries. Based on the three characteristic markers, FDA was performed on the different groups, which were then divided. The separation of strawberry samples from different origins using the three characteristic markers was found to be feasible. These findings help effectively understand the aroma and phenolic acid composition of strawberries and contribute to the development of strawberries with a pleasant fragrance and health benefits. Full article
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20 pages, 1505 KiB  
Article
Measuring the Phytochemical Richness of Meat: Effects of Grass/Grain Finishing Systems and Grapeseed Extract Supplementation on the Fatty Acid and Phytochemical Content of Beef
by Lucas Krusinski, Isabella C. F. Maciel, Stephan van Vliet, Muhammad Ahsin, Guanqi Lu, Jason E. Rowntree and Jenifer I. Fenton
Foods 2023, 12(19), 3547; https://doi.org/10.3390/foods12193547 - 24 Sep 2023
Cited by 2 | Viewed by 28480
Abstract
Grass-finished beef (GFB) can provide beneficial bioactive compounds to healthy diets, including omega-3 polyunsaturated fatty acids (n-3 PUFAs), conjugated linoleic acid (CLA), and secondary bioactive compounds, such as phytochemicals. The objective of this study was to compare fatty acids (FAs), micronutrients, [...] Read more.
Grass-finished beef (GFB) can provide beneficial bioactive compounds to healthy diets, including omega-3 polyunsaturated fatty acids (n-3 PUFAs), conjugated linoleic acid (CLA), and secondary bioactive compounds, such as phytochemicals. The objective of this study was to compare fatty acids (FAs), micronutrients, and phytochemicals of beef fed a biodiverse pasture (GRASS), a total mixed ration (GRAIN), or a total mixed ration with 5% grapeseed extract (GRAPE). This was a two-year study involving fifty-four Red Angus steers (n = 54). GFB contained higher levels of n-3 PUFAs, vitamin E, iron, zinc, stachydrine, hippuric acid, citric acid, and succinic acid than beef from GRAIN and GRAPE (p < 0.001 for all). No differences were observed in quantified phytochemicals between beef from GRAIN and GRAPE (p > 0.05). Random forest analysis indicated that phytochemical and FA composition of meat can predict cattle diets with a degree of certainty, especially for GFB (5.6% class error). In conclusion, these results indicate that GFB contains higher levels of potentially beneficial bioactive compounds, such as n-3 PUFAs, micronutrients, and phytochemicals, compared to grain-finished beef. Additionally, the n-6:n-3 ratio was the most crucial factor capable of separating beef based on finishing diets. Full article
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12 pages, 1260 KiB  
Article
Application of Static Headspace GC-MS Method for Selective 1,4-Dioxane Detection in Food Additives
by Myung-Chan Kim, Su-Yeon Park, Seo-Yeon Kwon, Yu-Kyeong Kim, Yeong-In Kim, Yong-Soo Seo, Sueng-Mok Cho, Eui-Cheol Shin, Jin Hong Mok and Yang-Bong Lee
Foods 2023, 12(17), 3299; https://doi.org/10.3390/foods12173299 - 2 Sep 2023
Viewed by 1481
Abstract
Efficient detection methods must be developed for 1,4-dioxane due to its suspected status as a human carcinogen, which is highly mobile in food and environmental resources. In this regard, this experiment has been conducted to develop reliable and selective detection and measurement methods [...] Read more.
Efficient detection methods must be developed for 1,4-dioxane due to its suspected status as a human carcinogen, which is highly mobile in food and environmental resources. In this regard, this experiment has been conducted to develop reliable and selective detection and measurement methods by using static headspace (SH) isolation, followed by gas chromatography–mass spectrometry (GC-MS). A new method was developed for determining the spiked 1,4-dioxane contents in a polyethylene glycol 600 (PEG 600). The optimal condition for SH-GC-MS was discussed. The representative ions of 1,4-dioxane and 1,4-dioxane-d8 in the SIM mode of MS are 88 and 96, respectively, and the peaks of the SIM mode were separated and confirmed. The linear range for the method covers 0.25 to 100 mg/L with a coefficient of determination (R2)  ≥  0.999. The method applicability was demonstrated by spike recovery across a variety of food additives (i.e., chlorine bitartrate, choline chloride, polysorbate 20 and 60, and PEG 1000). All spike recovery from the tested samples was in the range of 89.50–102.68% with a precision of 0.44–11.22%. These findings suggest a new analytical method for food safety inspection, and could be applicable for ensuring the safety of foods and environmental and public health on a broad scale. Full article
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14 pages, 1304 KiB  
Article
A Predictive Model to Correlate Amino Acids and Aromatic Compounds in Calabrian Honeys
by Sonia Carabetta, Rosa Di Sanzo, Salvatore Fuda, Adele Muscolo and Mariateresa Russo
Foods 2023, 12(17), 3284; https://doi.org/10.3390/foods12173284 - 1 Sep 2023
Cited by 1 | Viewed by 949
Abstract
To better understand the biochemistry of the organoleptic properties of honey influencing its commercial value, a predictive model for correlating amino acid profiles to aromatic compounds was built. Because the amino acid composition of different varieties of honey plays a key role as [...] Read more.
To better understand the biochemistry of the organoleptic properties of honey influencing its commercial value, a predictive model for correlating amino acid profiles to aromatic compounds was built. Because the amino acid composition of different varieties of honey plays a key role as a precursor of specific aroma bouquets, it is necessary to relate the amino acid typesetting to aromatic molecules. A selection of unifloral honeys produced in Calabria, South Italy, were used, and a new methodology based on the use of HILIC-UHPLC-ESI-MS/MS and HS-SPME-GC-MS combined with multivariate processing has been developed. This study, carried out for the first time on honey, shows its excellent potential as a modern analytical tool for a rapid multicomponent analysis of food-quality indicators. Data obtained showed strong positive linear correlations between aldehydes and isoleucine, valine, leucine, and phenylalanine. Furans are correlated with isoleucine, leucine, and phenylalanine; hydrocarbons with serine, glutamic acid, and aspartic acid; and ketones with serine, alanine, glutamine, histidine, asparagine, and lysine. Alcohols were more associated with tyrosine than esters with arginine. Proline, tryptophan, and threonine showed poor correlations with all the classes of aroma compounds. Full article
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17 pages, 3052 KiB  
Article
Differences and Similarities in Lipid Composition, Nutritional Value, and Bioactive Potential of Four Edible Chlorella vulgaris Strains
by Tatiana Maurício, Daniela Couto, Diana Lopes, Tiago Conde, Rita Pais, Joana Batista, Tânia Melo, Marisa Pinho, Ana S. P. Moreira, Mafalda Trovão, Ana Barros, Helena Cardoso, Joana Silva, Pedro Domingues and M. Rosário Domingues
Foods 2023, 12(8), 1625; https://doi.org/10.3390/foods12081625 - 12 Apr 2023
Cited by 3 | Viewed by 2182
Abstract
The microalga Chlorella vulgaris is a popular food ingredient widely used in the industry, with an increasing market size and value. Currently, several edible strains of C. vulgaris with different organoleptic characteristics are commercialized to meet consumer needs. This study aimed to compare [...] Read more.
The microalga Chlorella vulgaris is a popular food ingredient widely used in the industry, with an increasing market size and value. Currently, several edible strains of C. vulgaris with different organoleptic characteristics are commercialized to meet consumer needs. This study aimed to compare the fatty acid (FA) and lipid profile of four commercialized strains of C. vulgaris (C-Auto, C-Hetero, C-Honey, and C-White) using gas- and liquid-chromatography coupled to mass-spectrometry approaches, and to evaluate their antioxidant and anti-inflammatory properties. Results showed that C-Auto had a higher lipid content compared to the other strains and higher levels of omega-3 polyunsaturated FAs (PUFAs). However, the C-Hetero, C-Honey, and C-White strains had higher levels of omega-6 PUFAs. The lipidome signature was also different between strains, as C-Auto had a higher content of polar lipids esterified to omega-3 PUFAs, while C-White had a higher content of phospholipids with omega-6 PUFAs. C-Hetero and C-Honey showed a higher content of triacylglycerols. All extracts showed antioxidant and anti-inflammatory activity, highlighting C-Auto with greater potential. Overall, the four strains of C. vulgaris can be selectively chosen as a source of added-value lipids to be used as ingredients in food and nutraceutical applications for different market needs and nutritional requirements. Full article
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