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Advanced Chromatographic, Spectroscopic, and Spectrometric Techniques in 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 (10 February 2023) | Viewed by 28188

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Prof. Dr. Marco Beccaria

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Department of Chemical, Pharmaceutical and Agricultural Sciences—DOCPAS, University of Ferrara, Ferrara, Italy
Interests: food chemistry; analytical chemistry; biosources; fat and oils; volatilomics; lipidomics
Special Issues, Collections and Topics in MDPI journals

Dr. Chiara De Luca

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Department of Chemical, Pharmaceutical and Agricultural Sciences – DOCPAS, University of Ferrara, Ferrara, Italy
Interests: analytical chemistry; analytical and preparative chromatography; purification of biomolecules; proteins and peptides

Special Issue Information

Dear Colleagues,

It is our great pleasure and honor to invite you to contribute to a Special Issue in Foods titled “Advanced Chromatographic, Spectroscopic, and Spectrometric Techniques in Food Analysis”.

Food and agricultural products comprise complex sample systems made by diverse chemical structures mixtures wherein macronutrients (carbohydrates, proteins, and lipids), together with water and numerous minor components can coexist. The functional properties of these substances, which are ruled by their molecular structure and interactions within the food system, and the amounts present define the characteristics and quality of food products. Due to the continuous improvement in analytical technologies, over the past 100 years, food analysis has significantly evolved, passing from “wet chemistry” laboratory methods to the application of advanced and high-throughput analytical methodologies. Pioneering developments in chromatographic, spectrophotometric, and spectrometric techniques have led to significant improvements in identification capability, as well as in analytical accuracy, precision, detection limits, and sample throughput, thereby expanding the practical range of food applications. This Special Issue focuses on the optimization and validation of advanced and innovative chromatographic, spectrophotometric, and spectrometric methodologies in food analysis, in particular for quality and authenticity purposes.

Dr. Marco Beccaria
Dr. Chiara De Luca
Guest Editors

Manuscript Submission Information

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

food quality and authenticity
food characterization
chromatography
spectrophotometry
spectroscopy
hyphenated analytical techniques
macronutrients
minor components

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Published Papers (10 papers)

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19 pages, 12632 KiB

Open AccessArticle

A Study of the Interactions of Heavy Metals in Dairy Matrices Using Fourier Transform Infrared Spectroscopy, Chemometric, and In Silico Analysis

by Alfredo C. Benítez-Rojas, María E. Jaramillo-Flores, Orlando Zaca-Moran, Israel Quiroga-Montes and Raúl J. Delgado-Macuil

Foods 2023, 12(9), 1919; https://doi.org/10.3390/foods12091919 - 8 May 2023

Cited by 1 | Viewed by 2437

Abstract

Heavy metals are among the toxic substances longest recognized by man. Today, due to the myriad sources of exposure, such as contaminated water, food, or air, they have become a major public health problem. This work presents the effects manifested in the infrared spectrum behavior caused by the presence of Cd²⁺, Cr⁶⁺, and Pb²⁺ at different concentrations in three different matrices: water, casein, and milk; observing that the spectral modifications in the regions of different vibrational modes of nucleophilic groups such as -OH, COO- and NH₂ depending on the nature of the metal and its concentration. These findings were correlated in-silico using optimized models in Gabedit software and structural optimization was performed with MOPAC 2016 showing stable structures between the metals and Gln, Hys, Glu, and Phe of casein. By applying chemometrics (Principal Component Analysis), it was possible to observe a good correlation between the experimental data and to discriminate between the type of metal, the matrix that contains it, and the concentration could be represented through linear models that showed adjustments with a value of r² ≥ 0.95. Full article

(This article belongs to the Special Issue Advanced Chromatographic, Spectroscopic, and Spectrometric Techniques in Food Analysis)

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15 pages, 2204 KiB

Open AccessArticle

Establishment and Validation of Fourier Transform Infrared Spectroscopy (FT–MIR) Methodology for the Detection of Linoleic Acid in Buffalo Milk

by Zhiqiu Yao, Pei Nie, Xinxin Zhang, Chao Chen, Zhigao An, Ke Wei, Junwei Zhao, Haimiao Lv, Kaifeng Niu, Ying Yang, Wenna Zou and Liguo Yang

Foods 2023, 12(6), 1199; https://doi.org/10.3390/foods12061199 - 12 Mar 2023

Cited by 1 | Viewed by 2166

Abstract

Buffalo milk is a dairy product that is considered to have a higher nutritional value compared to cow’s milk. Linoleic acid (LA) is an essential fatty acid that is important for human health. This study aimed to investigate and validate the use of Fourier transform mid-infrared spectroscopy (FT-MIR) for the quantification of the linoleic acid in buffalo milk. Three machine learning models were used to predict linoleic acid content, and random forest was employed to select the most important subset of spectra for improved model performance. The validity of the FT-MIR methods was evaluated in accordance with ICH Q2 (R1) guidelines using the accuracy profile method, and the precision, the accuracy, and the limit of quantification were determined. The results showed that Fourier transform infrared spectroscopy is a suitable technique for the analysis of linoleic acid, with a lower limit of quantification of 0.15 mg/mL milk. Our results showed that FT-MIR spectroscopy is a viable method for LA concentration analysis. Full article

(This article belongs to the Special Issue Advanced Chromatographic, Spectroscopic, and Spectrometric Techniques in Food Analysis)

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24 pages, 4610 KiB

Open AccessArticle

Analytical Purity Determinations of Universal Food-Spice Curcuma longa through a QbD Validated HPLC Approach with Critical Parametric Predictors and Operable-Design’s Monte Carlo Simulations: Analysis of Extracts, Forced-Degradants, and Capsules and Tablets-Based Pharmaceutical Dosage Forms

by Hamdoon A. Mohammed, Dhafer S. Alsahabi, Amira M. Hegazy, Riaz A. Khan and Adel M. Ahmed

Foods 2023, 12(5), 1010; https://doi.org/10.3390/foods12051010 - 27 Feb 2023

Cited by 3 | Viewed by 2113

Abstract

Applications of analytical quality by design (QbD) approach for developing HPLC (High Performance Liquid Chromatography) methods for food components assays, and separations of complex natural product mixtures, are still limited. The current study developed and validated, for the first time, a stability-indicating HPLC method for simultaneous determinations of curcuminoids in Curcuma longa extracts, tablets, capsules, and curcuminoids’ forced degradants under different experimental conditions. Towards separation strategy, critical method parameters (CMPs) were defined as the mobile phase solvents’ percent-ratio, the pH of the mobile phase, and the stationary-phase column temperature, while the peaks resolution, retention time, and the number of theoretical plates were recognized as the critical method attributes (CMAs). Factorial experimental designs were used for method development, validation, and robustness evaluation of the procedure. The Monte Carlo simulation evaluated the developing method’s operability, and that ensured the concurrent detections of curcuminoids in natural extracts, commercial-grade pharmaceutical dosage-forms, and the forced degradants of the curcuminoids in a single mixture. The optimum separations were accomplished using the mobile phase, consisting of an acetonitrile–phosphate buffer (54:46 v/v, 0.1 mM) with 1.0 mL/min flow rate, 33 °C column temperature, and 385 nm wavelength for UV (Ultra Violet) spectral detections. The method is specific, linear (R2 ≥ 0.999), precise (% RSD < 1.67%), and accurate (% recovery 98.76–99.89%), with LOD (Limit of Detection) and LOQ (Limit of Quantitation) at 0.024 and 0.075 µg/mL for the curcumin, 0.0105 µg/mL and 0.319 µg/mL for demethoxycurcumin, and 0.335 µg/mL and 1.015 µg/mL for the bisdemethoxycurcumin, respectively. The method is compatible, robust, precise, reproducible, and accurately quantifies the composition of the analyte mixture. It exemplifies the use of the QbD approach in acquiring design details for developing an improved analytical detection and quantification method. Full article

(This article belongs to the Special Issue Advanced Chromatographic, Spectroscopic, and Spectrometric Techniques in Food Analysis)

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15 pages, 2439 KiB

Open AccessArticle

Hydrophobic Mesoporous Silica-Coated Solid-Phase Microextraction Arrow System for the Determination of Six Biogenic Amines in Pork and Fish

by Mengfei Chen, Hangzhen Lan, Daodong Pan and Tao Zhang

Foods 2023, 12(3), 578; https://doi.org/10.3390/foods12030578 - 28 Jan 2023

Cited by 8 | Viewed by 2027

Abstract

In this study, a functionalized mesoporous silica-coated solid-phase microextraction (SPME) Arrow system was developed for the enrichment of six biogenic amines (BAs) from pork and fish samples before gas chromatographic separation with a mass spectrometer as a detector. MCM-41 was utilized as the substrate material and thereby functionalized by titanate and sodium dodecyl sulfate to adjust its surface acidity and hydrophobicity, respectively. The functionalized MCM-41 (named as MCM-T-H) was coated on a bare SPME Arrow using the dipping method and polyacrylonitrile was used as the adhesive. The extraction capacity and selectivity of the MCM-T-H-SPME Arrow for six kinds of derivatized BAs were studied and compared with commercial SPME Arrows. Experimental parameters, e.g., sample volume, derivatization reagent amount, extraction time, and desorption time, which have a dramatic effect on SPME Arrow pretreatment, were optimized. Acidity enhanced MCM-T-H coating showed a much higher affinity to derivatized BAs compared to a commercial SPME Arrow in terms of extraction capacity. In addition, hydrophobicity modification significantly reduced the interference of water molecules on the interaction between MCM-T-H and the derivatized BAs. The MCM-T-H-SPME Arrow showed efficient separation and enrichment capacity for derivatized BAs from complex matrices and therefore, the sample pretreatment time was saved. According to the experimental results, the optimal condition was to add 10 μL derivatization reagent to a 10 mL sample and maintain an agitation speed of 1250 r min⁻¹. The MCM-T-H-SPME showed excellent reproducibility (RSD < 9.8%) and fast adsorption kinetics (30 min) and desorption kinetics (5 min) for derivatized BAs under optimal conditions. In summary, the MCM-T-H-SPME Arrow based method was employed for accurate monitoring of the variations of BAs in pork and fish, and good results were achieved. Full article

(This article belongs to the Special Issue Advanced Chromatographic, Spectroscopic, and Spectrometric Techniques in Food Analysis)

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21 pages, 1519 KiB

Open AccessArticle

Comprehensive Chemical Characterization of Chia (Salvia hispanica L.) Seed Oil with a Focus on Minor Lipid Components

by Marianna Oteri, Giovanni Bartolomeo, Francesca Rigano, Juan Aspromonte, Emanuela Trovato, Giorgia Purcaro, Paola Dugo, Luigi Mondello and Marco Beccaria

Foods 2023, 12(1), 23; https://doi.org/10.3390/foods12010023 - 21 Dec 2022

Cited by 11 | Viewed by 3762

Abstract

A comprehensive chemical characterization of different lipid components, namely fatty acid composition after derivatization in fatty acid methyl esters (FAMEs), triacylglycerols (TAGs), phospholipids (PLs), free fatty acids (FFAs), sterols, carotenoids, tocopherols, and polyphenols in Chia seed oil, obtained by Soxhlet extraction, was reported. Reversed phase liquid chromatography (RP-LC) coupled to UV and mass spectrometry (MS) detectors was employed for carotenoids, polyphenols, and TAGs determination; normal phase-LC in combination with fluorescence detector (FLD) was used for tocopherols analysis; PL and FFA fractions were investigated after a rapid solid phase extraction followed by RP-LC-MS and NanoLC coupled to electron ionization (EI) MS, respectively. Furthermore, gas chromatography (GC)-flame ionization (FID) and MS detectors were used for FAMEs and sterols analysis. Results demonstrated a significant content of bioactive compounds, such as the antioxidant tocopherols (22.88 µg mL⁻¹), and a very high content of essential fatty acids (81.39%), namely α-linolenic (62.16%) and linoleic (19.23%) acids. In addition, for the best of authors knowledge, FFA profile, as well as some carotenoid classes has been elucidated for the first time. The importance of free fatty acids in vegetable matrices is related to the fact that they can be readily involved in metabolic processes or biosynthetic pathways of the plant itself. For a fast and reliable determination of this chemical class, a very innovative and sensitive NanoLC-EI-MS analytical determination was applied. Full article

(This article belongs to the Special Issue Advanced Chromatographic, Spectroscopic, and Spectrometric Techniques in Food Analysis)

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22 pages, 2537 KiB

Open AccessArticle

Integrated Strategy for Informative Profiling and Accurate Quantification of Key-Volatiles in Dried Fruits and Nuts: An Industrial Quality Control Perspective

by Andrea Caratti, Simone Squara, Federico Stilo, Sonia Battaglino, Erica Liberto, Irene Cincera, Giuseppe Genova, Nicola Spigolon, Carlo Bicchi and Chiara Cordero

Foods 2022, 11(19), 3111; https://doi.org/10.3390/foods11193111 - 6 Oct 2022

Cited by 2 | Viewed by 1900

Abstract

Edible nuts and dried fruits, usually traded together in the global market, are one of the cornerstones of the Mediterranean diet representing a source of essential nutrients and bioactives. The food industry has an interest in the selection of high-quality materials for new product development while also matching consumers’ expectations in terms of sensory quality. In this study, walnuts (Juglans regia), almonds (Prunus dulcis), and dried pineapples (Ananas comosus) are selected as food models to develop an integrated analytical strategy for the informative volatile organic compounds (VOCs) quali- and quantitative profiling. The study deals with VOCs monitoring over time (12 months) and in the function of storage conditions (temperature and atmosphere).VOCs are targeted within those: (i) with a role in the product’s aroma blueprint (i.e., key-aromas and potent odorants); (ii) responsible for sensory degradation (i.e., rancidity); and/or (iii) formed by lipid autoxidation process. By accurate quantitative determination of volatile lipid oxidation markers (i.e., hexanal, heptanal, octanal, nonanal, decanal, (E)-2-heptenal, (E)-2-octenal, (E)-2-nonenal) product quality benchmarking is achieved. The combination of detailed VOCs profiling by headspace solid phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS) and accurate quantification of rancidity markers by multiple headspace-SPME (MHS-SPME) answers many different questions about shelf-life (i.e., aroma, storage stability, impact of temperature and storage atmosphere, rancidity level), while providing reliable and robust data for long-range studies and quality controls. The quantification associated with HS-SPME profiling is demonstrated and critically commented on to help the industrial research in a better understanding of the most suitable analytical strategies for supporting primary materials selection and new product development. Full article

(This article belongs to the Special Issue Advanced Chromatographic, Spectroscopic, and Spectrometric Techniques in Food Analysis)

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9 pages, 553 KiB

Open AccessArticle

Analysis of Cobalamin (Vit B12) in Ripened Cheese by Ultra-High-Performance Liquid Chromatography Coupled with Mass Spectrometry

by Giulia Rampazzo, Elisa Zironi, Giampiero Pagliuca and Teresa Gazzotti

Foods 2022, 11(18), 2745; https://doi.org/10.3390/foods11182745 - 7 Sep 2022

Cited by 2 | Viewed by 2880

Abstract

The analysis of natural cobalamins in dairy products still represents an analytical challenge. The matrix’s complexity, low concentration level, light sensitivity, and binding to proteins are just some of the aspects that make their quantification a difficult goal to achieve. Vitamin B12 plays a fundamental role in human nutrition, and its intake is closely linked to a diet that includes the consumption of food of animal origin. In the current literature, few studies have been carried out on the quantitation of cobalamin in ripened cheeses. A sensitive, selective, and robust ultra-high-performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS) method was developed, validated, and applied on ripened cheeses from different species (cow, sheep, and goat) purchased from local Italian markets, highlighting species-dependent differences in vitamin B12 concentrations. The vitamin B12 extraction procedure was performed by converting all cobalamins to the cyanocobalamin form. Furthermore, solid-phase extraction was used for matrix clean-up and analyte preconcentration. The proposed method showed good performance in terms of linearity, sensitivity, reproducibility, and repeatability. The mean vitamin B12 content ranged from <LOQ to 38.9 ng/g. Sheep cheese showed the highest concentrations of vitamin B12, with a mean content of 29.0 ng/g. Full article

(This article belongs to the Special Issue Advanced Chromatographic, Spectroscopic, and Spectrometric Techniques in Food Analysis)

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13 pages, 2100 KiB

Open AccessArticle

Simultaneous Detection and Analysis of Free Amino Acids and Glutathione in Different Shrimp

by Yinzhe Jin, Minhua Xu, Yingshan Jin, Shanggui Deng, Ningping Tao and Weiqiang Qiu

Foods 2022, 11(17), 2599; https://doi.org/10.3390/foods11172599 - 26 Aug 2022

Cited by 10 | Viewed by 2485

Abstract

An amino acid analyzer method for the simultaneous determination of 20 free amino acids (FAAs) and glutathione (GSH) in Penaeus vannamei (PV), Penaeus vannamei, Penaeus hidulis (PH) and Penaeus japonicus (PJ) were developed. The effects of different concentrations of trichloroacetic acid (TCA) and ethanol on the extraction of free amino acids were investigated, and 120 g·L⁻¹ TCA was found to be ideal. The target analytes were eluted in sodium citrate buffer B1 (pH = 3.3) containing 135 mL·L⁻¹ ethanol and 1 mol·L⁻¹ sodium hydroxide (7 mL) and at the optimizing conversion time of sodium citrate buffer B2 (pH = 3.2) and sodium citrate buffer B3 (pH = 4.0) of 5.6 min, and the effective separation was achieved within 29.5 min. The developed method showed good linearity (R² ≥ 0.9991) in the range of 1–250 µg·mL⁻¹ with good intra-day and inter-day precision (relative standard deviations ≤ 2.38%) and spike recovery (86.42–103.64%). GSH and cysteine were used to identify marine prawn and freshwater shrimp. Hydroxyproline and serine were used to distinguish PV and Macrobrachium nipponense (MN) from others, respectively. The highest content of the total FAAs was found in PV, and principal component analysis revealed that PV had the highest comprehensive score for FAAs and GSH. Arginine was found to have the greatest influence on shrimp flavor. Full article

(This article belongs to the Special Issue Advanced Chromatographic, Spectroscopic, and Spectrometric Techniques in Food Analysis)

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12 pages, 2279 KiB

Open AccessArticle

Investigation of the Volatile Profile of Red Jujube by Using GC-IMS, Multivariate Data Analysis, and Descriptive Sensory Analysis

by Yening Qiao, Qinqin Chen, Jinfeng Bi, Xinye Wu, Xinwen Jin, Min Gou, Xinrui Yang and Giorgia Purcaro

Foods 2022, 11(3), 421; https://doi.org/10.3390/foods11030421 - 31 Jan 2022

Cited by 8 | Viewed by 2864

Abstract

The aroma characteristics of six red jujube cultivars (Jinchang—‘JC’, Junzao—‘JZ’, Huizao—‘HZ’, Qiyuexian—‘QYX’, Hetiandazao—‘HTDZ’, and Yuanzao—‘YZ’), cultivated in Xinjiang Province, China, were studied by E-nose and GC-IMS. The presence of acetoin, E-2-hexanol, hexanal, acetic acid, and ethyl acetate played an important role in the classification results. JC, JZ, HZ, and YZ were different from others, while QYX and HTDZ were similar to each other. HZ had the most abundant specific VOCs, including linalool, nonanoic acid, methyl myristoleate, 2-acetylfuran, 1-octen-3-one, E-2-heptenal, 2-heptenone, 7-octenoic acid, and 2-pentanone. HZ had higher intensity in jujube ID, floral, sweet, and fruity attributes. Correlation analysis showed that jujube ID (identity) might be related to phenylacetaldehyde and isobutanoic acid that formed by the transamination or dehydrogenation of amino acids; meanwhile, the sweet attribute was correlated with amino acids, including threonine, glutamic acid, glycine, alanine, valine, leucine, tyrosine, phenylalanine, lysine, histidine, and arginine. Full article

(This article belongs to the Special Issue Advanced Chromatographic, Spectroscopic, and Spectrometric Techniques in Food Analysis)

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32 pages, 3197 KiB

Open AccessEditor’s ChoiceReview

Current Developments of Analytical Methodologies for Aflatoxins’ Determination in Food during the Last Decade (2013–2022), with a Particular Focus on Nuts and Nut Products

by Andrea Schincaglia, Juan Aspromonte, Flavio A. Franchina, Tatiana Chenet, Luisa Pasti, Alberto Cavazzini, Giorgia Purcaro and Marco Beccaria

Foods 2023, 12(3), 527; https://doi.org/10.3390/foods12030527 - 24 Jan 2023

Cited by 11 | Viewed by 4398

Abstract

This review aims to provide a clear overview of the most important analytical development in aflatoxins analysis during the last decade (2013–2022) with a particular focus on nuts and nuts-related products. Aflatoxins (AFs), a group of mycotoxins produced mainly by certain strains of the genus Aspergillus fungi, are known to impose a serious threat to human health. Indeed, AFs are considered carcinogenic to humans, group 1, by the International Agency for Research on Cancer (IARC). Since these toxins can be found in different food commodities, food control organizations worldwide impose maximum levels of AFs for commodities affected by this threat. Thus, they represent a cumbersome issue in terms of quality control, analytical result reliability, and economical losses. It is, therefore, mandatory for food industries to perform analysis on potentially contaminated commodities before the trade. A full perspective of the whole analytical workflow, considering each crucial step during AFs investigation, namely sampling, sample preparation, separation, and detection, will be presented to the reader, focusing on the main challenges related to the topic. A discussion will be primarily held regarding sample preparation methodologies such as partitioning, solid phase extraction (SPE), and immunoaffinity (IA) related methods. This will be followed by an overview of the leading analytical techniques for the detection of aflatoxins, in particular liquid chromatography (LC) coupled to a fluorescence detector (FLD) and/or mass spectrometry (MS). Moreover, the focus on the analytical procedure will not be specific only to traditional methodologies, such as LC, but also to new direct approaches based on imaging and the ability to detect AFs, reducing the need for sample preparation and separative techniques. Full article

(This article belongs to the Special Issue Advanced Chromatographic, Spectroscopic, and Spectrometric Techniques in Food Analysis)

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