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Development of Highly Efficient Separation-Based Analytical Methods for Food Integrity Assurance

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A special issue of Separations (ISSN 2297-8739). This special issue belongs to the section "Analysis of Food and Beverages".

Deadline for manuscript submissions: closed (31 October 2023) | Viewed by 30373

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Prof. Dr. Yiyang Dong

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Guest Editor

College of Life Science and Technology, Beijing University of Chemical Technology, Beijing 100029, China
Interests: rubber analysis; food analysis; high performance liquid chromatography; capillary electrophoresis; mass spectrometry
Special Issues, Collections and Topics in MDPI journals

Prof. Dr. Yuwei Yuan

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Co-Guest Editor

Agricultural Products Quality and Nutrition Institute, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China
Interests: food analysis; risk assessment; stable isotope; trace element; food traceability and authenticity; IRMS; ICP-MS
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

In recent years, highly efficient separation-based analytical methods have played an increasingly important role in food integrity (authenticity, safety and quality) and assurance for public health. Remarkable advances have been achieved in the development and optimization of separation-based analytical methods, which is useful for both the precise analysis and reliable identification of various food pathogens, contaminants, adulterants, and other risk factors.

This Special Issue will include both well-drafted manuscripts providing an overview of the current knowledge of highly efficient separation-based analytical methods and analytical procedures, and experimental investigations utilizing novel techniques with advanced materials or instrumental devices to address specific analytical problems in food samples for food integrity analysis.

The aim of this Special Issue is to not only provide a general overview of the modern separation-based analytical methods used to analyze and identify various deleterious or risk factors of food integrity, but also to outline the current research trends in these methods, and to acquaint the scientific community with modern separation procedures and approaches, whether targeted or non-targeted, i.e., profiling or screening studies.

Prof. Dr. Yiyang Dong
Prof. Dr. Yuwei Yuan
Guest Editors

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

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Keywords

food integrity
food safety
food authenticity
food fraud
analytical separation
precise analysis
targeted determination
non-target screening
solid-phase microextraction
QuEChERS

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Published Papers (9 papers)

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Research

13 pages, 2861 KiB

Open AccessArticle

Analysis of Two Single and Three Double Long-Chain Quaternary Ammonium Compounds via Non-Aqueous Capillary Electrophoresis with Indirect Ultraviolet Detection

by Kai Yao, Ruoke Jiang, Ping Wang, Jing Zhang, Bing Shao and Xiaojing Ding

Separations 2023, 10(7), 387; https://doi.org/10.3390/separations10070387 - 1 Jul 2023

Cited by 2 | Viewed by 1608

Abstract

A novel method utilizing non-aqueous capillary electrophoresis (NACE) with indirect ultraviolet detection (IUD) has been developed for the analysis of five quaternary ammonium compounds (QACs). The QACs analyzed in this study include dodecyl trimethyl ammonium bromide, tetradecyl trimethyl ammonium bromide, dioctyl dimethyl ammonium chloride, octyldecyl dimethyl ammonium chloride and didecyl dimethy ammonium bromide. The separation process was carried out on an uncoated fused quartz capillary with a total length of 50.2 cm (effective length 40.0 cm) and a diameter of 50 μm. The separation buffer consisted of a mixture of MeOH/ACN (90:10, v/v) containing 2 mmol/L sodium acetate, 2 mmol/L trifluoroacetic acid (TFA) and 16 mmol/L dodecyl dimethyl benzyl ammonium chloride. The sample buffer utilized a mixture of MeOH/ACN (20:80, v/v) containing 2 mmol/L TFA. During analysis, a separation voltage of 7 kV was applied, resulting in a current of approximately 2.3 μA. The detection wavelength was set at 214 nm to ensure optimal sensitivity. Under optimal conditions, the method exhibited excellent performance characteristics, with a limit of detection of 0.5 mg/L and a limit of quantitation of 5.0 mg/L for the five QACs. Linear calibration curves were obtained in a concentration range of 5.0 to 100.0 mg/L, with correlation coefficients exceeding 0.999 for all compounds. The recoveries of the five QACs ranged from 92.3% to 114.7%, with relative standard deviations below 7.4%. To assess the applicability of the NACE-IUD method, 17 commercially available samples were successfully analyzed. The results confirmed the suitability of the method for accurate determination of the five QACs in disinfectant products. Notably, this method offers an environmentally friendly approach for the analysis of these QACs. Full article

(This article belongs to the Special Issue Development of Highly Efficient Separation-Based Analytical Methods for Food Integrity Assurance)

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16 pages, 3311 KiB

Open AccessArticle

Geographical Origin Authentication of Edible Chrysanthemum morifolium Ramat. (Hangbaiju) Using Stable Isotopes

by Hanyi Mei, Jing Nie, Shu Wang, Yongzhi Zhang, Chunlin Li, Shengzhi Shao, Shanshan Shao, Karyne M. Rogers and Yuwei Yuan

Separations 2023, 10(5), 287; https://doi.org/10.3390/separations10050287 - 3 May 2023

Cited by 5 | Viewed by 1460

Abstract

Chrysanthemum morifolium Ramat., known as Hangbaiju (HBJ), is a high-value edible, medicinal product where the flowers are infused in hot water and drunk as tea. Its quality and efficacy are closely related to its geographical origin. Consequently, it is vulnerable to fraudulent substitution by other lower-value Chrysanthemum products. In this study, cultivation (variety and different growth stages) and isotopic fractionation between the flower, stem, and leaf were studied. Samples from four different HBJ varieties were characterized using stable isotopes (δ¹³C, δ¹⁵N, δ²H, δ¹⁸O, %C, and %N) across three producing regions in Zhejiang province, China. The results showed that there were no significant differences in stable isotopic compositions for different HBJ varieties, but there were significant differences for different plant tissues (flower, stem, leaf, etc.). Furthermore, the stable isotopic composition altered dramatically at different growth stages. The δ¹⁵N (r = 0.6809) and δ²H (r = 0.6102) correlations between stems and leaves (SL) and flowers (F) of HBJ were relatively good, the δ¹³C correlation (r = 0.2636) between SL and F was weak, but δ¹⁸O correlation (r = 0.01) had almost no correlation. A supervised multivariate statistical model (partial least squares discriminant analysis, PLS-DA) was used to discriminate three different producing regions with high accuracy (66.7%, 66.7%, and 100%, respectively). Our findings show that stable isotopes combined with multivariate statistical analysis provide an effective method for the geographical identification of HBJ. Full article

(This article belongs to the Special Issue Development of Highly Efficient Separation-Based Analytical Methods for Food Integrity Assurance)

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14 pages, 3018 KiB

Open AccessArticle

Extraction of Organochlorine Pesticides from Porous Membrane Packed Dried Fish Samples: Method Development and Greenness Evaluation

by Muhammad Sajid and Khalid Alhooshani

Separations 2023, 10(4), 233; https://doi.org/10.3390/separations10040233 - 1 Apr 2023

Cited by 2 | Viewed by 1741

Abstract

In this work, ultrasound-assisted solvent extraction was utilized for extraction of organochlorine pesticides from membrane-protected dried fish samples. The dried fish samples were packed inside a porous membrane bag which was immersed in a solvent and subjected to ultrasonication. After the extraction process, the sample-containing bag was separated from the extract. Since samples were packed inside the membrane, their separation did not require centrifugation or filtration. Moreover, the complex components of the biota matrix may also retain inside the porous membrane bag, alleviating the requirement of extract cleanup before analysis. The parameters that can affect the ultrasound-assisted solvent extraction of membrane-protected dried fish samples were suitably optimized. These parameters include the extraction solvent and its volume, the sample amount, ultrasound intensity and extraction time. Under the optimum extraction conditions, good linearity was achieved for all the tested organochlorine pesticides, with the coefficients of determination (R²) higher than 0.9922 for the linear ranges from 5–1000, 10–1000 and 20–1000 ng/g. The values of intra-day and inter-day relative standard deviations were ≤13.8%. The limit of detection ranged from 1.5 to 6.8 ng/g. The spiked relative recoveries were in the range of 87.3–104.2%. This method demonstrated excellent figures of merit and could find potential applications in routine analytical laboratories. Finally, the greenness of this method was evaluated using the green analytical procedure index and analytical greenness calculator metrics. Full article

(This article belongs to the Special Issue Development of Highly Efficient Separation-Based Analytical Methods for Food Integrity Assurance)

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11 pages, 969 KiB

Open AccessArticle

A Validated HPLC-RID Method for Quantification and Optimization of Total Sugars: Fructose, Glucose, Sucrose, and Lactose in Eggless Mayonnaise

by Mrityunjay Tiwari, Sandesh Mhatre, Tejas Vyas, Arohi Bapna and Govindarajan Raghavan

Separations 2023, 10(3), 199; https://doi.org/10.3390/separations10030199 - 14 Mar 2023

Cited by 6 | Viewed by 11485

Abstract

Mayonnaise is an oil-in-water emulsion containing 70–80% finely dispersed droplets of oil in a continuous phase of water. Since mayonnaise has a sour and acidic taste, its sugar profile is barely noticed and thus often disregarded. However, today, there are various variants of mayonnaise available on the market; hence, it is crucial to understand their mono- and disaccharide profile, in order to determine the precise total sugar composition. The traditional methods of sugar analysis available, such as titration, can only quantify sucrose and are unable to differentiate between mono- and disaccharides. The aim of this study was to develop and validate a method for the quantification of total sugars, including fructose, glucose, sucrose, and lactose, in eggless mayonnaise, using a high performance liquid chromatography refractive index detector (HPLC-RID). Sugars were separated on an amino column with an oven temperature of 35 °C, using an isocratic solvent system consisting of a 75:25 v/v mixture of acetonitrile and HPLC water, at a 0.9 mL/min flow rate with RID. Method validation was performed for the linearity, specificity, precision, accuracy, LOD, LOQ, and robustness. A linearity for total sugars, with a regression coefficient of 0.9998, was obtained within the range of 0.05024 to 10.048 mg/mL. The relative standard deviation was less than 2.0% for the intra-day and inter-day precision. The accuracy was found to be 96.78–108.88% using a three-level recovery method. The LOD and LOQ were also found to be suitable. The samples used in this study contained 0.24–10.32% total sugars. The sucrose value obtained matched the label claim of the products and no significant differences were observed between results in a paired sample t-test. This showed the applicability of the proposed method for analyzing the sugar profile in a finished product. Routine analysis of total sugars in eggless mayonnaise and similar finished products can thus be performed using this technique, which was found to be simple, rapid, and reproducible. Full article

(This article belongs to the Special Issue Development of Highly Efficient Separation-Based Analytical Methods for Food Integrity Assurance)

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14 pages, 2235 KiB

Open AccessArticle

Experimental Design Assisted HPLC/UV and LC-MS/MS for Simultaneous Determination of Selected Veterinary Antibiotics in Broiler Chicken

by Mohamed A. Abdelshakour, Aziza E. Mostafa, Ghada M. Hadad, Dalia M. Hamed, Omayma M. El-Darder, Alaa El-Gindy, Roaa M. Khinkar, Mohammed M. Aldurdunji, Samar S. Murshid and Randa A. Abdel Salam

Separations 2022, 9(12), 427; https://doi.org/10.3390/separations9120427 - 10 Dec 2022

Viewed by 2328

Abstract

Antibiotics are used in the poultry industry to treat and prevent diseases. Their frequent use resulted in the appearance of antibiotic residuals in poultry meat, which is considered a serious public health issue. Among frequently used antibiotics are cefotaxime (CTX), ciprofloxacin (CIP), colistin (CST), doxycycline (DOX), flumequine (FLU), sulfamethoxazole (SMZ), trimethoprim (TMP) and tylosin (TYL). This study aimed to develop an optimized and validated method for concurrent estimation of the eight antibiotics in broiler chicken samples based on an easy extraction method followed by HPLC-UV and LC/MS/MS analysis. An experimental design was used for the optimization of the extraction procedure. Optimal conditions for separation were determined by using a central composite design after studying (1) mobile phase initial concentration, (2) column temperature, and (3) flow rate. The method was validated on the bases of ICH guidelines. The detection limits ranged from 3 to 5 µg kg⁻¹ for HPLC- UV and ranged from 0.01 to 0.05 µg kg⁻¹ for LC/MS/MS, while quantification limits ranged from 10 to 16 µg kg⁻¹ for HPLC- UV and ranged from 0.01 to 0.11 µg kg⁻¹ for LC/MS/MS. The chromatographic techniques were utilized for the analysis of spiked broiler chicken samples at a concentration range from 30 to 300 µg kg⁻¹) for HPLC-UV and 0.01–20 µg kg⁻¹ for LC/MS/MS. The proposed methods were used for quantification of the residues of the studied antibiotics in real broiler samples obtained from local supermarkets in Ismailia governorate, Egypt. The detected levels of residual antibiotics were within the permissible limits. Full article

(This article belongs to the Special Issue Development of Highly Efficient Separation-Based Analytical Methods for Food Integrity Assurance)

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14 pages, 1287 KiB

Open AccessArticle

Towards a Better Quantification of Cyanotoxins in Fruits and Vegetables: Validation and Application of an UHPLC-MS/MS-Based Method on Belgian Products

by Wannes Hugo R. Van Hassel, Julien Masquelier, Mirjana Andjelkovic and Andreja Rajkovic

Separations 2022, 9(10), 319; https://doi.org/10.3390/separations9100319 - 20 Oct 2022

Cited by 7 | Viewed by 2109

Abstract

Vegetables and fruits can potentially accumulate cyanotoxins after water contaminated with cyanobacteria is used for irrigation. We developed and validated an analytical method to quantify eight microcystin congeners (MCs) and nodularin (NOD) using ultra high-performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS) in three different matrices. Strawberries, carrots and lettuce are selected as model matrices to represent the fruits/berries, leafy and root vegetables, sequentially. The validation of a UHPLC-MS/MS method in the strawberry matrix is novel. Matrix effects are observed in all three matrices. Our methodology uses matrix-matched calibration curves to compensate for the matrix effect. The implementation of our method on 103 samples, containing nine different sorts of fruits and vegetables from the Belgian market, showed no presence of MCs or NOD. However, the recoveries of our quality controls showed the effectiveness of our method, illustrating that the use of this method in future research or monitoring as well as in official food controls in fruit and vegetable matrices is valid. Full article

(This article belongs to the Special Issue Development of Highly Efficient Separation-Based Analytical Methods for Food Integrity Assurance)

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11 pages, 1576 KiB

Open AccessArticle

Comparative Analysis with GC–MS of Fatty Acids and Volatile Compounds of Taraxacum kok-saghyz Rodin and Taraxacum officinale as Edible Resource Plants

by Na Zhang, Tianyan Chen, Shuang Ye, Shunkai Gao and Yiyang Dong

Separations 2022, 9(10), 314; https://doi.org/10.3390/separations9100314 - 15 Oct 2022

Cited by 7 | Viewed by 2339

Abstract

Taraxacum kok-saghyz Rodin (TKS) is a potential edible resource plant that is rich in inulin, lipid, protein and other active ingredients. In this study, HS-SPME/GC–MS was used to analyze volatile compounds (VCs) and profile the fatty acids in TKS roots and leaves, and the results were compared with those from Taraxacum officinale (TO). A total of 105 and 107 VCs were detected in the leaves and roots of seven dandelion samples (three TKS and four TO), amongst which the main VCs were ethyl tetradecanoate, ethyl linolenate, ethyl linoleate, dihydroactinidiolide, ethyl palmitate, β-ionone, 3,5-octadien-2-one, β-ionone 5,6-epoxide, geranyl acetone, benzaldehyde, safranal, 2-Pentylfuran, farnesene and β-elemene. Linoleic acid and linolenic acid were the dominant fatty acids in seven dandelion samples, and the ratio of unsaturated to saturated fatty acids was larger than 4. Principal component analysis showed that the differences in VCs and fatty acid levels between different dandelion samples mainly came from different places of origin, while the differences between different varieties in the same place of origin was minor; i.e., the VCs and fatty acid levels of TKS and TO collected from the same place were basically similar. Full article

(This article belongs to the Special Issue Development of Highly Efficient Separation-Based Analytical Methods for Food Integrity Assurance)

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12 pages, 3012 KiB

Open AccessArticle

An Aptamer Affinity Column for Extraction of Four Aminoglycoside Antibiotics from Milk

by Liping Zhao, Xiaoqian Jiang, Xiaoling Xu, Nan Wang, Xinjie Wang, Ruiqi Yang, Xiangyang Liu, Zheng Liu and Yunxia Luan

Separations 2022, 9(10), 267; https://doi.org/10.3390/separations9100267 - 26 Sep 2022

Cited by 2 | Viewed by 1938

Abstract

This article introduces the aptamer affinity column (AAC) with nucleic acid aptamer as an affinity ligand for the extraction of four aminoglycoside antibiotics (AGs). The AAC was prepared by loading the aptamer functionalized Sepharose into an extraction column, which was conjugated by covalent binding between NHS-activated Sepharose and amino-modified aptamers with a coupling time of 2 h. After the sample solution flowed through the AAC, the AGs were retained because of the affinity between the AGs and aptamer, then AGs were eluted and analyzed by UPLC-MS/MS. Under the optimized conditions, the maximum adsorption of AGs on the AAC could reach 8.0 μg. Moreover, the proposed AAC could be reused more than 20 times. The resultant AAC that conjugated with the aptamer was successfully applied in the enrichment and purification of four AGs in a milk sample and good recovery results in the range of 83.3–98.8% were obtained (with RSD in the range of 0.6–5.8%). The proposed AAC for recognition of multi-target AGs exhibited good enrichment and purification effects, showing great application potential for targets with their related aptamers. Full article

(This article belongs to the Special Issue Development of Highly Efficient Separation-Based Analytical Methods for Food Integrity Assurance)

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12 pages, 678 KiB

Open AccessEditor’s ChoiceArticle

HPLC-MS, GC and NMR Profiling of Bioactive Lipids of Human Milk and Milk of Dairy Animals (Cow, Sheep, Goat, Buffalo, Camel, Red Deer)

by Kirill Lagutin, Andrew MacKenzie, Stephen Bloor, Dawn Scott and Mikhail Vyssotski

Separations 2022, 9(6), 145; https://doi.org/10.3390/separations9060145 - 7 Jun 2022

Cited by 14 | Viewed by 4076

Abstract

For non-bovine milks, information regarding bioactive lipids is fragmented, unreliable or unavailable. The purpose of the current study was to analyse bioactive lipids in the milk of dairy animals using modern analytical methods to achieve the most reliable results. Bioactive lipids in human milk were also analysed and used as a reference. A suite of modern analytical methods was employed, namely High Performance Liquid Chromatography-Mass Spectrometry (HPLC-MS), Gas Chromatography (GC) and Nuclear Magnetic Resonance (NMR). The total lipid content was determined, and phospholipid, fatty acid, neutral glycosphingolipids and ganglioside (GM3 and GD3) levels were measured. Lipid classes in selected milks were reliably characterised for the first time, including gangliosides in deer, camel and sheep; cerebrosides in deer, camel and buffalo; plasmalogens in deer, buffalo and goat and phospholipids in deer. Our study demonstrated the advantage of utilising a range of analytical techniques in order to characterise a diverse set of bioactive lipids. Full article

(This article belongs to the Special Issue Development of Highly Efficient Separation-Based Analytical Methods for Food Integrity Assurance)

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