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Processes
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Applications of Chromatographic Separation Techniques in Food and Chemistry—Second Edition
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Applications of Chromatographic Separation Techniques in Food and Chemistry—Second Edition

A special issue of Processes (ISSN 2227-9717). This special issue belongs to the section "Separation Processes".

Deadline for manuscript submissions: 10 May 2025 | Viewed by 6559

Special Issue Editor

Prof. Dr. Alina Pyka-Pająk

E-Mail Website
Guest Editor
Department of Analytical Chemistry, Faculty of Pharmaceutical Sciences in Sosnowiec, Medical University of Silesia in Katowice, Jagiellońska 4, 41-200 Sosnowiec, Poland
Interests: liquid chromatography; spectrophotometry; densitometry; organic compounds analysis; QSAR; QSRR; QSPR; pharmaceutical analysis; purity of pharmaceutical preparations
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

This is the second volume of the successful Special Issue we launched, titled "Applications of Chromatographic Separation Techniques in Food and Chemistry". In the first volume, we published 23 articles. (https://www.mdpi.com/journal/processes/special_issues/Chromatographic_Separation_Techniques).

Chromatographic techniques are by far the most powerful and versatile methods available to the modern analyst. Because of their good separation capacity, various chromatographic methods combined with modern detection systems are able to quickly separate very complicated mixtures into their individual components in a single-step process and are also capable of the simultaneous quantitative determination of each constituent.

Currently, chromatography is an extremely versatile technique which allows for the rapid separation of gases and volatile substances using gas chromatography, involatile chemicals, and materials of extremely high molecular weight using liquid chromatography, and, if necessary, very inexpensively using thin-layer chromatography coupled with densitometry. Therefore, chromatographic analyses are a widespread research method used in virtually all industries, also involving food processing as well as chemical synthesis. They allow for the detection of even trace amounts of substances in the finished product, which in turn gives the possibility of assessing the meticulous quality control of food products or the purity of newly synthesized bioactive molecules as potential new drug candidates, as well as others.

This Special Issue, focused on “Applications of Chromatographic Separation Techniques in Food and Chemistry”, aims to curate novel advances in the development and application of chromatographic separation techniques in food and chemical analyses. Topics of interest for this Special Issue include, but are not limited to, the following:

  • Chromatographic techniques used in ascertaining food quality and authenticity;
  • Chromatographic analysis of food additives, including food preservatives, antioxidants, sweeteners, colors, etc.;
  • Basic research and applications of chromatographic techniques in chemistry;
  • Application of chromatographic techniques in pharmaceutical analysis;
  • The development of new chromatographic methods in the analysis of food and chemical compounds, including bioactive molecules;
  • Chromatography as a separation technique useful in the chemical process industry; for analysis, isolation, and purification of various chemical compounds as the components of small- and large-scale production.

Original research papers as well as reviews related to the abovementioned areas are most welcome.

Prof. Dr. Alina Pyka-Pająk
Guest Editor

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. Processes is an international peer-reviewed open access monthly 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 2400 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

  • chromatographic techniques (GC, HPLC, TLC, TLC-densitometry)
  • food components
  • food quality
  • chemical analysis
  • analysis of bioactive compounds
  • pharmaceutical analysis
  • separation techniques

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Further information on MDPI's Special Issue polices can be found here.

Published Papers (6 papers)

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Research

15 pages, 1383 KiB  
Article
Affordable and Reliable RP-HPLC Method for Verapamil Hydrochloride Quantification in Rabbit Plasma for Pharmacokinetics
by Raja Navamanisubramanian, Shanmuganathan Seetharaman, Abimanyu Sugumaran, Mona Y. Alsheikh, Ibrahim A. Naguib and Mohammed Gamal
Processes 2024, 12(10), 2211; https://doi.org/10.3390/pr12102211 - 11 Oct 2024
Viewed by 586
Abstract
Background: Existing bioanalytical methods for verapamil hydrochloride (VH) are often complex, requiring advanced instrumentation and specialized expertise, which limits their use in resource-constrained laboratories. Aim: The goal of this study is to fill this gap by developing a simplified, robust RP-HPLC-UV approach for [...] Read more.
Background: Existing bioanalytical methods for verapamil hydrochloride (VH) are often complex, requiring advanced instrumentation and specialized expertise, which limits their use in resource-constrained laboratories. Aim: The goal of this study is to fill this gap by developing a simplified, robust RP-HPLC-UV approach for the estimation of verapamil hydrochloride in rabbit plasma. Designed to enhance accuracy and precision while minimizing sample preparation challenges, this method addresses existing limitations by providing an affordable and reliable alternative for laboratories lacking sophisticated instrumentation. Methods: The bioanalytical method was implemented on C-18 stationary phase (5 μ, 250 × 4.6 mm) using acetonitrile/0.1% tetrahydrofuran (THF) in water (80:20, in volume) as the liquid system at a 1 mL/min flow speed, employing carvedilol as an internal standard. Results: The reported retention times of verapamil hydrochloride and carvedilol were ~7.64 and 4.69 min, respectively, at sufficiently high system suitability standards. The linearity of the bioanalytical approach can be seen between 0.025 and 5.0 µg/mL (r2 = 0.9991). The findings indicated that there was no matrix influence in terms of accuracy (≥98.96 ± 2.68%), intra- and inter-day precision (≤3.68%), recovery (101.98 ± 2.76%), and procedure efficiency (100.65 ± 1.82%). Benchtop, long-term, and short-term stability investigations all revealed that the verapamil hydrochloride in the bio-samples was stable. The pharmacokinetic parameters (Cmax—3.47 µg/mL; Tmax—1.59 h) were studied from time-dependent plasma concentrations of verapamil hydrochloride estimated after 40 mg oral dosing in New Zealand white rabbits. Conclusions: The developed bioanalytical method provided easier quantitative analysis of verapamil hydrochloride from rabbit plasma and was effectively used in a pharmacokinetic investigation of an oral bolus. The reliable performance of this method under practical conditions positions it as a crucial tool for advancing pharmacokinetic studies across various research environments. Full article
(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry—Second Edition)
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24 pages, 4071 KiB  
Article
Analysis of Aromatic Fraction of Sparkling Wine Manufactured by Second Fermentation and Aging in Bottles Using Different Types of Closures
by Patricia Jové, Glòria Mateu-Figueras, Jessica Bustillos and Josep Antoni Martín-Fernández
Processes 2024, 12(10), 2165; https://doi.org/10.3390/pr12102165 - 4 Oct 2024
Viewed by 794
Abstract
This study aimed to evaluate the impact of different closures used in second fermentation on the aromatic fraction of sparkling wine. Six types of closures (cork stoppers and screw caps) and 94 months of aging in a bottle were investigated. Headspace solid-phase microextraction [...] Read more.
This study aimed to evaluate the impact of different closures used in second fermentation on the aromatic fraction of sparkling wine. Six types of closures (cork stoppers and screw caps) and 94 months of aging in a bottle were investigated. Headspace solid-phase microextraction (HS-SPME) and thermal desorption (TD) procedures coupled to gas chromatography-mass spectrometry (GCMSMS) analysis were applied. The vectors containing the relative abundance of the volatile compounds are compositional vectors. The statistical analysis of compositional data requires specific techniques that differ from standard techniques. Overall, 101 volatile compounds were identified. HS-SPME extracted the highest percentage of esters, ketones and other compounds, while TD was a useful tool for the obtention of alcohol, acid, ether and alkane compounds. Esters were the most abundant family of compounds. Compositional data analysis, which was applied to study the impact of different closures used in bottle aging after second fermentation on the volatile composition of sparkling wine, concluded that there are differences in the relative abundance of certain volatile compounds between cork stoppers and screw-cap closures. Overall, the most abundant part in screw-cap closures was ethyl hexanoate, and it was ethyl octanoate in cork stoppers. Also, the proportional amount of dimethylamine was higher in screw-cap closures than cork stoppers relative to the entire sample. Full article
(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry—Second Edition)
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17 pages, 2695 KiB  
Article
Studies of TLC-Chromatographic Quantification of Astaxanthin in Dietary Supplements and Its Antioxidant Activity
by Iwona Dymek, Joanna Żandarek, Małgorzata Starek and Monika Dąbrowska
Processes 2024, 12(8), 1680; https://doi.org/10.3390/pr12081680 - 11 Aug 2024
Viewed by 1182
Abstract
Astaxanthin is a red carotenoid pigment known for its strong antioxidant and immune-supporting properties, which are higher than other carotenoids. The aim of this study was the qualitative and quantitative evaluation of dietary supplements containing astaxanthin. First, optimal conditions for conducting analyses using [...] Read more.
Astaxanthin is a red carotenoid pigment known for its strong antioxidant and immune-supporting properties, which are higher than other carotenoids. The aim of this study was the qualitative and quantitative evaluation of dietary supplements containing astaxanthin. First, optimal conditions for conducting analyses using the TLC technique with densitometric detection were developed. The mobile phase consisting of methanol: ethyl acetate: 1,4-dioxane (1:3:6 v/v/v) was selected, while the stationary phase consisted of Silica gel 60 F254. Densitometric detection was performed at 460 nm. Next, the validation process of the developed method was carried out according to the guidelines of the International Conference on Harmonization (ICH). The range of linearity tested was 0.0026–0.0100 µg/spot, and the determined LOD and LOQ values were 0.85 and 2.57 ng/μL, respectively. The variation coefficient at the level of 4.75% proves good precision. The percentage of recovery was in the range of 95.25–104.94%. The obtained results confirmed the good accuracy of the method. Subsequently, quantitative analyses of the preparations were carried out. Analysis of dietary supplements showed significant deviations from the declared astaxanthin content. Astaxanthin solutions were stable in alkaline environments and when exposed to light and oxidizing substances; however, the substance degraded in acidic environments. The performed antioxidant capacity tests confirmed the high antioxidant activity of astaxanthin. Full article
(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry—Second Edition)
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9 pages, 1801 KiB  
Communication
The Determination of LogP of Anticoagulant Drugs with High-Performance Thin-Layer Chromatography
by Matylda Resztak and Andrzej Czyrski
Processes 2024, 12(8), 1599; https://doi.org/10.3390/pr12081599 - 30 Jul 2024
Viewed by 986
Abstract
The lipophilicity of a substance is an important physicochemical parameter for the pharmacological activity of a drug. In the current study, high-performance thin-layer chromatography was applied to determine the LogP values of the following anticoagulant drugs: warfarin, acenocoumarol, clopidogrel, and prasugrel. The mobile [...] Read more.
The lipophilicity of a substance is an important physicochemical parameter for the pharmacological activity of a drug. In the current study, high-performance thin-layer chromatography was applied to determine the LogP values of the following anticoagulant drugs: warfarin, acenocoumarol, clopidogrel, and prasugrel. The mobile phase was a mixture of acetonitrile and water in mixed proportions. The content of acetonitrile varied from 50% to 80% in 5% increments. The partition coefficients were calculated with the regression curve Rm0 = f(LogP) based on the compounds with known lipophilicity. The highest LogP was observed for warfarin and the lowest for prasugrel. Full article
(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry—Second Edition)
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15 pages, 3133 KiB  
Article
Development and Validation of Ultra-Performance Liquid Chromatography (UPLC) Method for Simultaneous Quantification of Hydrochlorothiazide, Amlodipine Besylate, and Valsartan in Marketed Fixed-Dose Combination Tablet
by Doaa Hasan Alshora, Abdelrahman Y. Sherif and Mohamed Abbas Ibrahim
Processes 2024, 12(6), 1259; https://doi.org/10.3390/pr12061259 - 19 Jun 2024
Viewed by 970
Abstract
Fixed-dose combination therapy is considered a practical approach in the treatment of various diseases, as it can simultaneously target different mechanisms of action that achieve the required therapeutic efficacy through a synergistic effect. A combination of hydrochlorothiazide (HTZ), amlodipine (AMD), and valsartan (VLS) [...] Read more.
Fixed-dose combination therapy is considered a practical approach in the treatment of various diseases, as it can simultaneously target different mechanisms of action that achieve the required therapeutic efficacy through a synergistic effect. A combination of hydrochlorothiazide (HTZ), amlodipine (AMD), and valsartan (VLS) has been created for the treatment of hypertension. Therefore, the aim of this study was to develop an optimized UPLC method for the simultaneous quantification of this combination. A DoE at a level of 32 was used to investigate the effects of column temperature (20, 30, and 40 °C) and formic acid concentration (0.05, 0.15, and 0.25%) on the retention time of each active pharmaceutical ingredient (API), the peak area, and the peak symmetry, as well as the resolution between HTZ-AMD and AMD-VLS peaks. The optimized analytical method was validated and used to extract the three APIs from the marketed product. The optimized analytical condition with a column temperature of 27.86 °C and a formic acid concentration of 0.172% showed good separation of the three APIs in 1.62 ± 0.006, 3.59 ± 0.002, and 3.94 ± 0.002 min for HTZ, AMD, and VST, respectively. The developed method was linear with the LOQ for a HTC, AMD, and VST of 0.028, 0.038, and 0.101 ppm, respectively. Moreover, the developed assay was sustainable and robust, with an RSD % of less than 2%. The application of this method in the extraction of HTZ, AMD, and VST from the Exforge® marketed product showed good separation with a measurable drug content of 23.5 ± 0.7, 9.68 ± 0.1, and 165.2 ± 5.2 mg compared to the label claims of 25/10/160 for HTZ, AMD, and VST, respectively. Full article
(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry—Second Edition)
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15 pages, 5125 KiB  
Article
Comparison of the Limit of Detection of Paracetamol, Propyphenazone, and Caffeine Analyzed Using Thin-Layer Chromatography and High-Performance Thin-Layer Chromatography
by Katarzyna Bober-Majnusz and Alina Pyka-Pająk
Processes 2024, 12(6), 1153; https://doi.org/10.3390/pr12061153 - 3 Jun 2024
Viewed by 961
Abstract
TLC (thin-layer chromatography) and HPTLC (high-performance thin-layer chromatography) in normal (NP) and reversed (RP) phase systems were combined with densitometry to analyze caffeine, propyphenazone, and paracetamol. This work aims to check whether comparable limit of detection (LOD) values can be obtained on TLC [...] Read more.
TLC (thin-layer chromatography) and HPTLC (high-performance thin-layer chromatography) in normal (NP) and reversed (RP) phase systems were combined with densitometry to analyze caffeine, propyphenazone, and paracetamol. This work aims to check whether comparable limit of detection (LOD) values can be obtained on TLC and HPTLC plates. Analyses were performed on five (NP) or four (RP) different stationary phases (chromatographic plates), testing, in both cases, three mobile phases. It is shown that by using both TLC and HPTLC plates, it is possible to develop chromatographic conditions that enable the detection of compounds analyzed in amounts ranging from a dozen to several dozen µg/spot. In the RP system, lower LOD values for all tested compounds were obtained using TLC than HPTLC. However, performing analyses in the NP, similar (of the same order) LOD values were obtained for caffeine, propyphenazone, and paracetamol when using both TLC and HPTLC plates. For example, during the NP-HPTLC analysis using silica gel 60F254 plates (#1.05548) and mobile phase B (n-hexane—acetone—ammonia, 25:25:0.5, v/v/v), LOD values for caffeine, propyphenazone, and paracetamol were 0.010, 0.046, and 0.030 μg/spot, respectively. During NP-TLC analysis using silica gel 60F254 (#1.05554 plates) and the mobile phase C (chloroform—toluene—ethyl acetate—methanol—80% acetic acid, 18:18:7.5:6:0.3, v/v), the values of LOD were 0.054, 0.029, and 0.016 μg/spot, respectively. During RP-TLC analysis using TLC RP-18F254 plates (#1.05559) and mobile phase F (methanol-water, 40:10, v/v), the LOD values were 0.019, 0.024, and 0.053 μg/spot, respectively. Therefore, for economical reasons, TLC plates should be recommended for analyses of caffeine, propyphenazone, and paracetamol, which are several times cheaper than HPTLC plates. Full article
(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry—Second Edition)
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