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Development of Analytical Methods in the Field of Food Analysis

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

Deadline for manuscript submissions: closed (31 March 2023) | Viewed by 22948

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Dr. Gianfranco Picone

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Department of Agricultural and Food Sciences (DISTAL), University of Bologna, 47521 Cesena, Italy
Interests: metabolomics; HR-NMR; foodomics; nutrimetabolomics; chemometrics
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Dear Colleagues,

Any product intended for human consumption needs to be rigorously tested, and because foodstuffs are ingested, the testing is often especially crucial to prevent any potential health issues. Thus, food analysis is a very important branch of analytical chemistry, as it provides information about the chemical composition, processing, quality control, and contamination of foodstuffs, ensuring compliance with food and trade laws. For this reason, it impacts both the economic and medical aspects of modern societies. The development of analytical methods in food matrices, as well as the understanding of how the food matrix influences nutrients’ bioaccessibility, has always been difficult due to the large variety of their physicochemical properties. In terms of the techniques that are used to name a few common examples, the range of instruments includes nuclear magnetic resonance (NMR) spectroscopy, gas chromatography (GC), atomic absorption spectroscopy (AAS), and high-performance liquid chromatography (HPLC). The choice of technique(s) depends on what foodstuff is being analyzed, what is being analyzed within the foodstuff, and the reasons for the analysis, which can change analyte structure and extraction efficiencies because of different processing procedures throughout preparation and distribution.

Furthermore, the multiplexing trend, which means the simultaneous detection of multiple analytes at the same time, requires the development of more appropriate sample preparation methods, as well as instruments that take into account such factors as sustainability, green chemistry, and operator intervention.

This Special Issue is open to submissions that explore the development of analytical methods in the field of food analysis, which also includes topics such as in vitro digestion and nanotechnology in food safety and quality assessment. Original works and reviews are welcomed.

Dr. Gianfranco Picone
Guest Editor

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Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

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. Foods 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 2900 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

analytical methods
food security
mass spectrometry
raman spectroscopy
nmr spectroscopy
chromatography
solid-phase microextraction
sampling and sample preparation
nanomaterials in diagnostics
green chemistry
in vitro digestion
metabolomics

Published Papers (11 papers)

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Research

16 pages, 1135 KiB

Open AccessArticle

Simultaneous Determination of Multiple Contaminants in Chicken Liver Using Dispersive Liquid-Liquid Microextraction (DLLME) Detected by LC-HRMS/MS

by Belete Eshetu Gebreyohannes, Simiso Dube and Mathew Muzi Nindi

Foods 2023, 12(13), 2594; https://0-doi-org.brum.beds.ac.uk/10.3390/foods12132594 - 04 Jul 2023

Viewed by 1084

Abstract

Simultaneous determination of a mixture of food contaminants, including pesticides, sulphonamides, fluoroquinolones, anthelmintics, and aflatoxin B1, in solid biological samples (chicken liver) by dispersive liquid-liquid microextraction/liquid chromatography-high resolution mass spectrometry (DLLME/LC-HRMS) is presented. Previous work focused on the application of DLLME to single-class contaminants. In this work, the DLLME extraction method has been extended to complex multiresidues in the biological matrix. The first part of this study was the selection of an appropriate solvent that enabled the dissolution of analytes from the chicken livers. The matrix-matched calibration curves showed good linearity in the range 0.5–50.0 µg kg⁻¹ for aflatoxin B1 and 50–500 µg kg⁻¹ for pesticides, fluoroquinolones, sulphonamides, and anthelmintics, with a coefficient of determination (R²) values of 0.9916–0.9967. The mean recoveries were in the range of 80.4–96.3%, and the relative standard deviation (RSD) values were in the range of 1.53–8.98%. The limit of detection (LOD) and the limit of quantification (LOQ) values were 0.03 µg kg⁻¹ and 0.09 µg kg⁻¹, respectively, for aflatoxin B1, and for pesticides, fluoroquinolones, sulphonamides, and anthelmintics, they were in the range of 0.011–1.197 µg kg⁻¹ and 0.150–2.579 µg kg⁻¹, respectively. The developed method was compared with the standard solid phase extraction (SPE) method, and there was no significant difference between the two methods. Full article

(This article belongs to the Special Issue Development of Analytical Methods in the Field of Food Analysis)

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17 pages, 2646 KiB

Open AccessArticle

Characterization of Flavor Profile of “Nanx Wudl” Sour Meat Fermented from Goose and Pork Using Gas Chromatography–Ion Mobility Spectrometry (GC–IMS) Combined with Electronic Nose and Tongue

by Xin Zhao, Jianying Feng, Luca Laghi, Jing Deng, Xiaofang Dao, Junni Tang, Lili Ji, Chenglin Zhu and Gianfranco Picone

Foods 2023, 12(11), 2194; https://0-doi-org.brum.beds.ac.uk/10.3390/foods12112194 - 30 May 2023

Cited by 7 | Viewed by 1843

Abstract

Sour meat is a highly appreciated traditional fermented product, mainly from the Guizhou, Yunnan, and Hunan provinces. The flavor profiles of sour meat from goose and pork were evaluated using gas chromatography–ion mobility spectrometry (GC–IMS) combined with an electronic nose (E-nose) and tongue (E-tongue). A total of 94 volatile compounds were characterized in fermented sour meat from both pork and goose using GC–IMS. A data-mining protocol based on univariate and multivariate analyses revealed that the source of the raw meat plays a crucial role in the formation of flavor compounds during the fermentation process. In detail, sour meat from pork contained higher levels of hexyl acetate, sotolon, heptyl acetate, butyl propanoate, hexanal, and 2-acetylpyrrole than sour goose meat. In parallel, sour meat from goose showed higher levels of 4-methyl-3-penten-2-one, n-butyl lactate, 2-butanol, (E)-2-nonenal, and decalin than sour pork. In terms of the odor and taste response values obtained by the E-nose and E-tongue, a robust principal component model (RPCA) could effectively differentiate sour meat from the two sources. The present work could provide references to investigate the flavor profiles of traditional sour meat products fermented from different raw meats and offer opportunities for a rapid identification method based on flavor profiles. Full article

(This article belongs to the Special Issue Development of Analytical Methods in the Field of Food Analysis)

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13 pages, 1066 KiB

Open AccessArticle

Development of Extraction Method for Determination of Saponins in Soybean-Based Yoghurt Alternatives: Effect of Sample pH

by Anastassia Bljahhina, Maria Kuhtinskaja and Tiina Kriščiunaite

Foods 2023, 12(11), 2164; https://0-doi-org.brum.beds.ac.uk/10.3390/foods12112164 - 27 May 2023

Cited by 1 | Viewed by 1722

Abstract

The number of plant-based dairy alternative products on the market is growing rapidly. In the case of soybean-based yoghurt alternatives, it is important to trace the content of saponins, the phytomicronutrients with a disputable health effect, which are likely to be responsible for the bitter off-taste of the products. We present a new sample extraction method followed by hydrophilic interaction liquid chromatography with mass spectrometric detection (HILIC-MS) for identifying and quantifying soyasaponins in soybean-based yoghurt alternatives. Soyasaponin Bb, soyasaponin Ba, soyasaponin Aa, and soyasaponin Ab were quantified using commercially available standard compounds and with asperosaponin VI as the internal standard. As the recoveries of soyasaponins were unacceptable in yoghurt alternatives at their natural acidic pH, the adjustment of pH was performed as one of the first steps in the sample extraction procedure to achieve the optimum solubility of soyasaponins. The validation of the method included the assessment of linearity, precision, limit of detection and limit of quantification (LOQ), recovery, and matrix effect. The average concentrations of soyasaponin Bb, soyasaponin Ba, soyasaponin Ab, and soyasaponin Aa in several measured soybean-based yoghurt alternatives utilising the developed method were 12.6 ± 1.2, 3.2 ± 0.7, 6.0 ± 2.4 mg/100 g, and below the LOQ, respectively. This method provides an efficient and relatively simple procedure for extracting soyasaponins from yoghurt alternatives followed by rapid quantification using HILIC-MS and could find a rightful application in the development of healthier and better-tasting dairy alternatives. Full article

(This article belongs to the Special Issue Development of Analytical Methods in the Field of Food Analysis)

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35 pages, 4531 KiB

Open AccessFeature PaperArticle

Low-Field Benchtop NMR Spectroscopy for Quantification of Aldehydic Lipid Oxidation Products in Culinary Oils during Shallow Frying Episodes

by Miles Gibson, Benita Claire Percival, Mark Edgar and Martin Grootveld

Foods 2023, 12(6), 1254; https://0-doi-org.brum.beds.ac.uk/10.3390/foods12061254 - 15 Mar 2023

Cited by 5 | Viewed by 1824

Abstract

Introduction: Toxic aldehydic lipid oxidation products (LOPs) arise from the thermo-oxidative deterioration of unsaturated fatty acids present in heated culinary oils when exposed to high-temperature frying episodes, and currently these effects represent a major public health concern. Objectives: In this study, we investigated the applications of low-field (LF), benchtop NMR analysis to detect and quantify toxic aldehyde species in culinary oils following their exposure to laboratory-simulated shallow frying episodes (LSSFEs) at 180 °C. Four culinary oils of variable fatty acid (FA) composition were investigated to determine the analytical capabilities of the LF NMR instrument. Oil samples were also analysed using a medium-field (400 MHz) NMR facility for comparative purposes. Results: Aldehydes were quantified as total saturated and total α,β-unsaturated classes. The time-dependent production of α,β-unsaturated aldehydes decreased in the order chia > rapeseed ≈ soybean > olive oils, as might be expected from their polyunsaturated and monounsaturated FA (PUFA and MUFA, respectively) contents. A similar but inequivalent trend was found for saturated aldehyde concentrations. These data strongly correlated with medium-field ¹H NMR data obtained, although LF-determined levels were significantly lower in view of its inability to detect or quantify the more minor oxygenated aldehydic LOPs present. Lower limit of detection (LLOD) values for this spectrometer were 0.19 and 0.18 mmol/mol FA for n-hexanal and trans-2-octenal, respectively. Aldehydic lipid hydroperoxide precursors of aldehydic LOPs were also detectable in LF spectra. Conclusions: We therefore conclude that there is scope for application of these smaller, near-portable NMR facilities for commercial or ‘on-site’ quality control determination of toxic aldehydic LOPs in thermally stressed frying oils. Full article

(This article belongs to the Special Issue Development of Analytical Methods in the Field of Food Analysis)

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16 pages, 706 KiB

Open AccessArticle

Quantitative Analysis of Oat (Avena sativa L.) and Pea (Pisum sativum L.) Saponins in Plant-Based Food Products by Hydrophilic Interaction Liquid Chromatography Coupled with Mass Spectrometry

by Anastassia Bljahhina, Dmitri Pismennõi, Tiina Kriščiunaite, Maria Kuhtinskaja and Eeva-Gerda Kobrin

Foods 2023, 12(5), 991; https://0-doi-org.brum.beds.ac.uk/10.3390/foods12050991 - 26 Feb 2023

Cited by 4 | Viewed by 2903

Abstract

This work presents the sample extraction methods for solid and liquid sample matrices for simultaneous quantification of oat (Avena sativa L.) and pea (Pisum sativum L.) saponins: avenacoside A, avenacoside B, 26-desglucoavenacoside A, and saponin B and 2,3-dihydro-2,5-dihydroxy-6-methyl-4H-pyran-4-one (DDMP) saponin, respectively. The targeted saponins were identified and quantified using a hydrophilic interaction liquid chromatography with mass spectrometric detection (HILIC-MS) method. The simple and high-throughput extraction procedure was developed for solid oat- and pea-based food samples. In addition, a very simple extraction procedure for liquid samples, without the need to use lyophilisation, was also implemented. Oat seed flour (U-¹³C-labelled) and soyasaponin Ba were used as internal standards for avenacoside A and saponin B, respectively. Other saponins were relatively quantified based on avenacoside A and saponin B standard responses. The developed method was tested and successfully validated using oat and pea flours, protein concentrates and isolates, as well as their mixtures, and plant-based drinks. With this method, the saponins from oat- and pea-based products were separated and quantified simultaneously within 6 min. The use of respective internal standards derived from U-¹³C-labelled oat and soyasaponin Ba ensured high accuracy and precision of the proposed method. Full article

(This article belongs to the Special Issue Development of Analytical Methods in the Field of Food Analysis)

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15 pages, 5233 KiB

Open AccessArticle

Effect of High Hydrostatic Pressure on the Metabolite Profile of Striped Prawn (Melicertus kerathurus) during Chilled Storage

by Qiuyu Lan, Silvia Tappi, Giacomo Braschi, Gianfranco Picone, Pietro Rocculi and Luca Laghi

Foods 2022, 11(22), 3677; https://0-doi-org.brum.beds.ac.uk/10.3390/foods11223677 - 17 Nov 2022

Cited by 2 | Viewed by 1220

Abstract

A variety of metabolites contribute to the freshness and taste characteristics of seafood. This study investigated the effects of high hydrostatic pressure (HHP; 400, 500, and 600 MPa) for 10 min) on the metabolome of striped prawn during chilled storage, in relation to microorganisms’ development. All treated samples showed lower viable counts throughout storage compared to the untreated counterparts. The limit of acceptability from a microbiological point of view was extended from 9 to as many as 35 days by 600 MPa treatment. Metabolites were quantified by ¹H-NMR through a targeted-untargeted metabolomic approach. Molecules linked to nucleotides’ degradation and amines’ anabolism suggested an overall freshness improvement granted by HHP. Notably, putrescine and cadaverine were detected only in untreated prawn samples, suggesting the inactivation of degradative enzymes by HHP. The concentration of molecules that influence umami perception was significantly elevated by HHP, while in untreated samples, the concentration of molecules contributing to a sour taste gradually increased during storage. As metabolomics was applied in its untargeted form, it allowed us to follow the overall set of metabolites related to HHP processing and storage, thus providing novel insights into the freshness and taste quality of striped prawn as affected by high hydrostatic pressure. Full article

(This article belongs to the Special Issue Development of Analytical Methods in the Field of Food Analysis)

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12 pages, 1062 KiB

Open AccessArticle

Development and Method Validation of Butyric Acid and Milk Fat Analysis in Butter Blends and Blended Milk Products by GC-FID

by Arunee Danudol and Kunchit Judprasong

Foods 2022, 11(22), 3606; https://0-doi-org.brum.beds.ac.uk/10.3390/foods11223606 - 12 Nov 2022

Cited by 3 | Viewed by 3045

Abstract

Butyric acid is a short-chain saturated fatty acid with four carbon atoms in its molecule. It is unique to butter made from cow’s milk and is an indicator to evaluate the quality of butter and milk products as stated in their ingredient labels. This study determined the milk fat content of butter blends and blended milk products by analyzing the content of butyric acid prepared as derivatives of methyl esters prior to injection into a gas chromatography flame ionization detector (GC–FID). Results revealed that this method had specificity, a linear relationship for concentration in the range of 0.04–1.60 mg/mL, a coefficient of determination (R²) > 0.999, an instrumental limit of detection (LOD) and a limit of quantitative analysis (LOQ) at 0.01% and 0.10% of total fat, respectively, and an instrumental working range of 0.10–3.60% of total fat. The results of a precision study using relative standard deviation (RSD) was 1.3%, while an accuracy study using the spiking method showed % recovery in the range of 98.2–101.9%. The method linearity range for milk fat analysis had a good linear correlation in the range of 3–100% of total fat (R² > 0.999). Results for method LOD and LOQ were 1% and 3% of total fat, respectively. This method also had good precision (1.3% RSD) and accuracy (99.6–100.1% recovery), which indicates reliability in terms of precision and accuracy. This method, therefore, can be used to check claims about the quality of blended butter and blended milk products to ensure consumer confidence in product quality. Full article

(This article belongs to the Special Issue Development of Analytical Methods in the Field of Food Analysis)

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12 pages, 1830 KiB

Open AccessArticle

Cheese Whey Milk Adulteration Determination Using Casein Glycomacropeptide as an Indicator by HPLC

by Ricardo Vera-Bravo, Angela V. Hernández, Steven Peña, Carolina Alarcón, Alix E. Loaiza and Crispín A. Celis

Foods 2022, 11(20), 3201; https://0-doi-org.brum.beds.ac.uk/10.3390/foods11203201 - 14 Oct 2022

Cited by 6 | Viewed by 1908

Abstract

Raw milk adulteration with cheese whey is a major problem that affects the dairy industry. The objective of this work was to evaluate the adulteration of raw milk with the cheese whey obtained from the coagulation process, with chymosin enzyme using casein glycomacropeptide (cGMP) as an HPLC marker. Milk proteins were precipitated with 24% TCA; with the supernatant obtained, a calibration curve was established by mixing raw milk and whey in different percentages, which were passed through a KW-802.5 Shodex molecular exclusion column. A reference signal, with a retention time of 10.8 min, was obtained for each of the different percentages of cheese whey; the higher the concentration, the higher the peak. Data analysis was adjusted to a linear regression model, with an R² of 0.9984 and equation to predict dependent variable (cheese whey percentage in milk) values. The chromatography sample was collected and analyzed by three tests: a cGMP standard HPLC analysis, MALDI-TOF spectrometry, and immunochromatography assay. The results of these three tests confirmed the presence of the cGMP monomer in adulterated samples with whey, which was obtained from chymosin enzymatic coagulation. As a contribution to food safety, the molecular exclusion chromatography technique presented is reliable, easy to implement in a laboratory, and inexpensive, compared with other methodologies, such as electrophoresis, immunochromatography, and HPLC-MS, thus allowing for the routine quality control of milk, an important product in human nutrition. Full article

(This article belongs to the Special Issue Development of Analytical Methods in the Field of Food Analysis)

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12 pages, 2649 KiB

Open AccessArticle

The Longer the Storage Time, the Higher the Price, the Better the Quality? A ¹H-NMR Based Metabolomic Investigation of Aged Ya’an Tibetan Tea (Camellia sinensis)

by Chenglin Zhu, Zhibo Yang, Li He, Xuan Lu, Junni Tang and Luca Laghi

Foods 2022, 11(19), 2986; https://0-doi-org.brum.beds.ac.uk/10.3390/foods11192986 - 25 Sep 2022

Cited by 6 | Viewed by 1608

Abstract

As an essential beverage beneficial for Tibetan people, Ya’an Tibetan tea has received scarce attention, particularly from the point of view of the characterization of its metabolome. The aim of the study is to systematically characterize the metabolome of Tibetan tea by means of untargeted ¹H-NMR. Moreover, the variations of its metabolome along ageing time are evaluated by taking advantage of univariate and multivariate analyses. A total of 45 molecules are unambiguously identified and quantified, comprising amino acids, peptides and analogues, carbohydrates and derivates, organic acids and derivates, nucleosides, nucleotides and catechins. The concentrations of amino acids, organic acids, carbohydrates and catechins are mainly determined by ageing time. The present study would serve as a reference guide for further work on the Ya’an Tibetan tea metabolome, therefore contributing to the related industries. Full article

(This article belongs to the Special Issue Development of Analytical Methods in the Field of Food Analysis)

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15 pages, 2032 KiB

Open AccessArticle

A New Electrochemical Method to Determine Tryptophan in Fruit Juices: Development and Validation

by Assefa Takele, José María Palacios-Santander and Miguel Palma

Foods 2022, 11(14), 2149; https://0-doi-org.brum.beds.ac.uk/10.3390/foods11142149 - 20 Jul 2022

Viewed by 1939

Abstract

Tryptophan (Trp) is an essential amino acid usually found in fruit juices. Its determination is necessary for food companies because of its relation to human health. In this work, a new electrochemical method based on sonogel–carbon electrodes (SNGCEs) was developed and validated using an ultra performance liquid chromatography (UPLC) method as a reference method for the determination of Trp in fruit juices. Cyclic voltammetry (CV), chronoamperometry, and differential pulse voltammetry (DPV) techniques were applied to investigate the oxidation of Trp on a previously polarized SNGCE surface in a Britton–Robinson (BR) buffer solution at pH 3.6. The operating conditions for electroanalysis were optimized using a Box–Behnken design (BBD), obtaining an oxidation peak for Trp at 0.749 V. The linear range for this method was from 0.1 to 5 mg/L. The intraday and interday precision, expressed as a relative standard deviation (RSD), were 3.1% and 2.7%, respectively. The average recovery was 99.01%, and the limit of detection and quantitation were 0.33 and 1.09 mg/L, respectively. Therefore, from the quality analytical parameters obtained, it can be concluded that the new electrochemical method can be successfully used for the routine analysis of Trp in fruit juices. As far as we are concerned, this is the first time that a methodology for Trp determination was performed in this kind of real food matrices. Full article

(This article belongs to the Special Issue Development of Analytical Methods in the Field of Food Analysis)

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15 pages, 2268 KiB

Open AccessArticle

An Integrative Glycomic Approach for Quantitative Meat Species Profiling

by Sean Chia, Gavin Teo, Shi Jie Tay, Larry Sai Weng Loo, Corrine Wan, Lyn Chiin Sim, Hanry Yu, Ian Walsh and Kuin Tian Pang

Foods 2022, 11(13), 1952; https://0-doi-org.brum.beds.ac.uk/10.3390/foods11131952 - 30 Jun 2022

Cited by 2 | Viewed by 2354

Abstract

It is estimated that food fraud, where meat from different species is deceitfully labelled or contaminated, has cost the global food industry around USD 6.2 to USD 40 billion annually. To overcome this problem, novel and robust quantitative methods are needed to accurately characterise and profile meat samples. In this study, we use a glycomic approach for the profiling of meat from different species. This involves an O-glycan analysis using LC-MS qTOF, and an N-glycan analysis using a high-resolution non-targeted ultra-performance liquid chromatography-fluorescence-mass spectrometry (UPLC-FLR-MS) on chicken, pork, and beef meat samples. Our integrated glycomic approach reveals the distinct glycan profile of chicken, pork, and beef samples; glycosylation attributes such as fucosylation, sialylation, galactosylation, high mannose, α-galactose, Neu5Gc, and Neu5Ac are significantly different between meat from different species. The multi-attribute data consisting of the abundance of each O-glycan and N-glycan structure allows a clear separation between meat from different species through principal component analysis. Altogether, we have successfully demonstrated the use of a glycomics-based workflow to extract multi-attribute data from O-glycan and N-glycan analysis for meat profiling. This established glycoanalytical methodology could be extended to other high-value biotechnology industries for product authentication. Full article

(This article belongs to the Special Issue Development of Analytical Methods in the Field of Food Analysis)

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