Applications of Chromatographic Separation Techniques in Food and Chemistry

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

Deadline for manuscript submissions: closed (15 January 2024) | Viewed by 66877

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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
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Co-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: drug analysis; instrumental methods; liquid chromatography; bioactive compounds; product quality; QSPR; QSAR
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

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 simultaneous quantitative determination of each constituent.

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

This Special Issue 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 include but are not limited to:

  • 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;
  • The development of new chromatographic methods in the analysis of food and chemical compounds, including bioactive molecules;
  • Chromatography as 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 areas mentioned above are most welcome.

Prof. Dr. Alina Pyka-Pająk
Dr. Małgorzata Dołowy
Guest Editors

Manuscript Submission Information

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Keywords

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

Published Papers (24 papers)

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Editorial

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5 pages, 181 KiB  
Editorial
Special Issue on “Applications of Chromatographic Separation Techniques in Food and Chemistry”
by Alina Pyka-Pająk
Processes 2024, 12(2), 304; https://doi.org/10.3390/pr12020304 - 31 Jan 2024
Viewed by 581
Abstract
Chromatographic techniques and methods are experiencing significant growth in various industries [...] Full article

Research

Jump to: Editorial, Review

13 pages, 1324 KiB  
Article
Determination of Five Phosphodiesterase-5 Inhibitors in Multiple Honey-Based Consumer Products by Chromatographic Technique in Rat Plasma
by Wael Abu Dayyih, Ammar A. Rasras, Mohammad Hailat, Rawan Karaki, Ahmad A. Deeb, Israa Al-Ani, Lina N. AlTamimi, Zainab Zakaraya, Sina M. Matalqah, Basim Mareekh, Enas Alkhader and Eyad S. M. Abu-Nameh
Processes 2023, 11(10), 3019; https://doi.org/10.3390/pr11103019 - 20 Oct 2023
Viewed by 824
Abstract
This study aimed to develop and verify a simple HPLC-based quantitative approach to simultaneously determine the phosphodiesterase-5 inhibitors (PDE5Is) sildenafil, vardenafil, udenafil, avanafil, and tadalafil in a tablet dosage form mixed with honey obtained form Jordanian market in rat plasma. PDE5Is block phosphodiesterase-5 [...] Read more.
This study aimed to develop and verify a simple HPLC-based quantitative approach to simultaneously determine the phosphodiesterase-5 inhibitors (PDE5Is) sildenafil, vardenafil, udenafil, avanafil, and tadalafil in a tablet dosage form mixed with honey obtained form Jordanian market in rat plasma. PDE5Is block phosphodiesterase-5 (PDE-5). This blockage, in turn, triggers vasodilation by phosphorylating downstream effector molecules. Chromatographic separation was performed on a HypersilTM C18 column (150 mm × 4.6 mm, 5 µm, Thermo Fisher Inc., Waltham, MA, USA). An acetonitrile:10% Triethylamine solution (57:43) at pH 5.5 (adjusted with orthophosphoric acid), 20 µL injection volume, 1 mL/min flow rate, 25 °C temperature, and eluent monitoring at 250 nm was used to execute the current approach. Linearity was observed in the 9.6–14.4 µg/mL concentration ranges for sildenafil, udenafil, avanafil, and tadalafil, and 2.4–3.6 µg/mL for vardenafil. Each dosage form was recovered within acceptable limits at three distinct concentrations, and the assay selectivity indicated no interference from the inactive substances in the formulation. Sildenafil, vardenafil, udenafil, avanafil, and tadalafil had retention times of 3.5, 4.3, 6.2, 9.7, and 12.8 min, respectively, and tadalafil was 12.8 min. The present analytical method is comprehensive and universal for measuring the five drugs. Such an analytical method can be routinely used to detect the combination of these drugs. Full article
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12 pages, 1709 KiB  
Article
Comprehensive Analysis of Phenolic Compounds, Carotenoids, and Antioxidant Activities in Lactuca sativa var. longifolia Cultivated in a Smart Farm System
by Jungwon Choi, Joonggeun An, Hak-Dong Lee, Woo Jung Kim, Sullim Lee and Sanghyun Lee
Processes 2023, 11(10), 2993; https://doi.org/10.3390/pr11102993 - 17 Oct 2023
Viewed by 843
Abstract
Smart farming is a promising strategy for future agriculture, and the global market for smart agriculture is growing rapidly. The aim of this study was to compare the quality of agricultural products based on their cultivation method. The components and antioxidant activities of [...] Read more.
Smart farming is a promising strategy for future agriculture, and the global market for smart agriculture is growing rapidly. The aim of this study was to compare the quality of agricultural products based on their cultivation method. The components and antioxidant activities of Lactuca sativa (LS) var. longifolia cultivated using conventional agriculture methods (CAMs) and smart farm agriculture methods (SAMs) were compared. ABTS+ and DPPH radical scavenging activity assays were performed to compare the antioxidant activities of LS grown using CAMs and SAMs. High-performance liquid chromatography with a reverse-phase column was employed to analyze the phenolic and carotenoid compounds. In both the SAM and the CAM, β-carotene was found to be the most abundant compound. LS grown using the CAM had high total polyphenol content and ABTS+ radical scavenging activity, while LS grown using the SAM had high individual phenolic content and DPPH radical scavenging activity. This study developed a new method of SAM and confirmed that SAM produces a higher quantity of phenolic compounds and total flavonoid contents than CAM in LS. This study also highlights the SAM’s functioning, gives crop quality inspection guidelines, and standardizes LS. The new SAM is effective for application in undeveloped urban spaces, is more convenient than the CAM, and represents a way to develop and manage LS quality. Full article
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18 pages, 2143 KiB  
Article
Development and Validation of Gas Chromatography–Mass Spectrometry Method for Quantification of Sibutramine in Dietary Supplements
by Vanya Rangelov Kozhuharov, Kalin Ivanov, Diana Karcheva-Bahchevanska, Natalia Prissadova and Stanislava Ivanova
Processes 2023, 11(8), 2337; https://doi.org/10.3390/pr11082337 - 03 Aug 2023
Cited by 1 | Viewed by 1344
Abstract
The use of dietary supplements (DSs) has dramatically increased in recent decades. However, around 20% of these products are reported to contain pharmacologically active undeclared compounds, most of which could expose consumers to serious side effects. According to recent data, some of the [...] Read more.
The use of dietary supplements (DSs) has dramatically increased in recent decades. However, around 20% of these products are reported to contain pharmacologically active undeclared compounds, most of which could expose consumers to serious side effects. According to recent data, some of the most commonly detected undeclared compounds are also considered doping and are prohibited by the World Anti-Doping Agency (WADA). One of the most frequently detected undeclared substances in DSs used for promoting weight loss is sibutramine. In 2011, all medicines containing sibutramine were urgently withdrawn from Europe and US markets because of serious side effects. In the present study, in order to detect and quantify sibutramine in DSs, a rapid, sensitive, and reliable gas chromatography with mass spectrometry (GC-MS) method was developed. The method was validated according to the ICH guidelines and demonstrated good linearity, accuracy, precision, and robustness. The limits of detection and quantification were 0.181 μg/mL and 0.5488 μg/mL, respectively. The method was applied to analyze 50 DSs promoting weight loss, fat burning, and performance enhancement. Sibutramine was detected in six of them in a range of 16.59–14,854.94 μg/per capsule. The high concentrations of sibutramine detected in some samples raise concerns about the potential health risks associated with the use of adulterated DSs. The proposed GC-MS method could be used successfully in the quality control of DSs or in different research programs, contributing to safety and the prevention of associated side effects. Full article
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13 pages, 1477 KiB  
Article
Simultaneous Analysis of Flumethasone Pivalate and Clioquinol in the Presence of Phenoxyethanol Preservative in Their Pharmaceuticals Using TLC and UHPLC Methods
by Faisal K. Algethami, Huda Salem AlSalem, Mohammed Gamal, Nada Nabil, Hala E. Zaazaa, Mohamed A. Ibrahim and Asmaa A. Mandour
Processes 2023, 11(7), 1888; https://doi.org/10.3390/pr11071888 - 23 Jun 2023
Cited by 1 | Viewed by 896
Abstract
Two novel separation methods have been presented for the concurrent assessment of flumethasone pivalate (FP) and clioquinol (CL) in their combinations in ear drop formulations or in the presence of phenoxyethanol preservative (PEP) in their cream formulations. The first method is an innovative [...] Read more.
Two novel separation methods have been presented for the concurrent assessment of flumethasone pivalate (FP) and clioquinol (CL) in their combinations in ear drop formulations or in the presence of phenoxyethanol preservative (PEP) in their cream formulations. The first method is an innovative thin-layer chromatographic (TLC) method. The optimal separation was accomplished via silica gel aluminum plates F254, with a mixture of benzene, ethyl acetate and formic acid (5:5:0.2, in volumes) as the mobile system. In Method II, a new ultra-high-performance liquid chromatographic method (UHPLC) with a photodiode array detector (PDA) was presented. A reversed-phase inertsil ODS 5 µm C 18 packed column (100 Å, 4.6 mm internal diameter (I.D.) × 50 mm) at 30 °C was employed. Elution was completed in 3 min. Unfortunately, greener solvents were tested as a mobile phase, but an asymmetric peak for CL was noted. In addition, the new UHPLC method has a priority over the old HPLC one by Sayed et al., 2014, in terms of quickness and avoiding interference from the PEP preservative. Concerning the TLC method, the novel TLC method has the advantage of preventing the interference of PEP. This paper represents the first analytical approach for the concurrent assay of FP and CL in the presence of the preservative phenoxyethanol in the cream formulation. Full article
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13 pages, 2413 KiB  
Article
Development and Validation of High-Performance Liquid Chromatography for Identification and Quantification of Phytoecdysteroids Ecdysterone and Turkesterone in Dietary Supplements
by Velislava Todorova, Kalin Ivanov, Diana Karcheva-Bahchevanska and Stanislava Ivanova
Processes 2023, 11(6), 1786; https://doi.org/10.3390/pr11061786 - 12 Jun 2023
Cited by 4 | Viewed by 2295
Abstract
Phytoecdysteroids are a group of naturally occurring ecdysteroid hormones found in certain plant families and used for centuries for their adaptogenic, tonifying, and antioxidant properties. Ecdysterone and turkesterone are the dominant phytoecdysteroids found in the plant species Rhaponticum carthamoides Willd., Cyanotis arachnoidea C.B.Clarke [...] Read more.
Phytoecdysteroids are a group of naturally occurring ecdysteroid hormones found in certain plant families and used for centuries for their adaptogenic, tonifying, and antioxidant properties. Ecdysterone and turkesterone are the dominant phytoecdysteroids found in the plant species Rhaponticum carthamoides Willd., Cyanotis arachnoidea C.B.Clarke and Ajuga turkestanica (Regel) Briq., and have been recognized for their adaptogenic potential and ability to enhance physical performance. However, over the past few years, supplementation with ecdysterone by professional athletes has raised some concerns about its safety and quality, leading to its inclusion in the World Anti-Doping Agency monitoring program. This study proposes a simple and reliable method for quality control of ecdysterone- and turkesterone-containing products using high-performance liquid chromatography (HPLC) analysis. The HPLC method is based on reversed-phase chromatography and gradient elution to achieve a superior separation of phytoecdysteroids. The method has been shown to qualify both phytoecdysteroids at low concentrations such as 10.98 μg/mL for ecdysterone and 11.43 μg/mL for turkesterone. This method could be successfully used in research programs and routine quality control of dietary supplements to ensure their safety in professional athletes’ nutrition. Full article
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12 pages, 2613 KiB  
Article
Development of a Zeolite H-ZSM-5-Based D-μSPE Method for the Determination of Organophosphorus Pesticides in Tea Beverages
by Bing Bai, Nan Wu, Haifeng Yang, Haiyan Liu, Xiaofen Jin, Lei Chen, Zhiying Huang, Changyan Zhou, Shouying Wang and Wenshuai Si
Processes 2023, 11(4), 1027; https://doi.org/10.3390/pr11041027 - 28 Mar 2023
Cited by 1 | Viewed by 979
Abstract
In this study, a novel dispersive micro-solid phase extraction (D-μSPE) technique with H-ZSM-5 zeolite as an adsorbent was developed for the determination of 21 trace pesticides in tea beverages. The adsorption and desorption of H-ZSM-5 zeolites were investigated based on structural characteristics and [...] Read more.
In this study, a novel dispersive micro-solid phase extraction (D-μSPE) technique with H-ZSM-5 zeolite as an adsorbent was developed for the determination of 21 trace pesticides in tea beverages. The adsorption and desorption of H-ZSM-5 zeolites were investigated based on structural characteristics and adsorption properties similar to those of H-beta zeolites. In combination with the properties of the adsorbates, it was explained that the adsorption reaction occurred on the microporous surface and mesopores of H-ZSM-5. Based on optimal parameters, the beverage samples were extracted by 50 mg of zeolite within 1 min. The zeolite was eluted with 2 mL of an acetonitrile-water mixture after separation, and the eluent was filtered prior to HPLC-MS/MS analysis. The D-μSPE protocol demonstrated acceptable accuracy and precision, with recoveries between 62.1% and 106.6% and relative standard deviations of 1.4% to 12.6%, as validated by analytical reliability. The correlation coefficient in the linear range of 0.2–50 ng·mL−1 was greater than 0.98, with limits of detection of 0.05–0.1 ng·mL−1 and limits of quantification of 0.1–0.2 ng·mL−1. The matrix effects ranged from 76.2% to 112.7%. The results indicate that the novel D-μSPE technique based on H-ZSM-5 is a rapid, simple, green and economical method for the determination of pesticide residues in tea beverages. The proposed method achieved simultaneously low adsorbent dosage, 20-fold enrichment factor, rapid pre-concentration in 12 min, minimal organic wastes, and effective reduction of matrix interference. Full article
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16 pages, 2279 KiB  
Article
Development and Optimization of Chromatographic Conditions for the Determination of Selected B Vitamins in Pharmaceutical Products
by Joanna Żandarek, Żaneta Binert-Kusztal, Małgorzata Starek and Monika Dąbrowska
Processes 2023, 11(3), 937; https://doi.org/10.3390/pr11030937 - 19 Mar 2023
Cited by 2 | Viewed by 2633
Abstract
Vitamins are a unit of organic chemical substances that are essential for the adequate working of the human body. Water-soluble B vitamins are involved in the regulation of many metabolic and regulatory processes. Due to the inability to synthesize endogenously, they must be [...] Read more.
Vitamins are a unit of organic chemical substances that are essential for the adequate working of the human body. Water-soluble B vitamins are involved in the regulation of many metabolic and regulatory processes. Due to the inability to synthesize endogenously, they must be supplied to the body with edibles or in the form of supplementation as drugs or dietary supplements. Maintaining the correct level of vitamins is extremely important in the treatment of various diseases. In the presented work, the qualitative and quantitative procedure of the assay of vitamins B1, B2, B5, B6 and B12 in pharmaceutical products by chromatographic technique coupled with densitometric detection was developed, optimized and validated. During the optimization process, TLC Silica gel 60 F254 plates were chosen as a suitable stationary, and the mixture consisted of chloroform: ethanol: water: glacial acetic acid (2:8:2:0.5 v/v/v/v) as a mobile phase. Densitometric detection was conducted at a maximum absorbance λ = 254 nm for vitamins B1, B2, B6 and B12 and λ = 550 nm for vitamin B5 (after dyeing with ninhydrin). In the next step, the developed procedure was validated in accordance with the ICH guidelines. The recorded correlation coefficients obtained in all tested concentrations of B vitamins, ranging from 0.9947 to 0.9996, confirmed good linearity. The method is characterized by good precision, RSD data ranging from 0.62 to 1.52% for direct precision and from 0.84 to 1.4% for intermediate precision. Accuracy was proven by a recovery test at three concentration levels, with values close to 100% with RSD less than 1%. The calculated LOD and LOQ data for all tested vitamins B1, B2, B5, B6 and B12 were belove 1 μg/spot. The developed method was then used to quantitatively and qualitatively assess the content of B vitamins in medicinal products and dietary supplements with satisfactory results. Full article
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14 pages, 2800 KiB  
Article
Development of a SPE-HPLC-PDA Method for the Quantification of Phthalates in Bottled Water and Their Gene Expression Modulation in a Human Intestinal Cell Model
by Vincenzo Ferrone, Pantaleone Bruni, Teresa Catalano, Federico Selvaggi, Roberto Cotellese, Giuseppe Carlucci and Gitana Maria Aceto
Processes 2023, 11(1), 45; https://doi.org/10.3390/pr11010045 - 25 Dec 2022
Cited by 3 | Viewed by 1667
Abstract
Phthalates are ubiquitous pollutants that are currently classified as endocrine disruptor chemicals causing serious health problems. As contaminants of food and beverages, they come into contact with the epithelium of the intestinal tract. In this work, a SPE-HPLC-PDA method for the determination of [...] Read more.
Phthalates are ubiquitous pollutants that are currently classified as endocrine disruptor chemicals causing serious health problems. As contaminants of food and beverages, they come into contact with the epithelium of the intestinal tract. In this work, a SPE-HPLC-PDA method for the determination of phthalates in water from plastic bottles was developed and validated according to the food and drug administration (FDA) guidelines. A chromatographic separation was achieved using a mobile phase consisting of ammonium acetate buffer 10 mM pH 5 (line A) and a mixture of methanol and iso-propanol (50:50 v/v, line B) using gradient elution. Several SPE cartridges and different pH values were investigated for this study, evaluating their performance as a function of recovery. Among these parameters, pH 5 combined with the SPE sep pack C18 cartridge showed the best performance. Finally, the proposed method was applied to the analysis of real samples, which confirmed the presence of phthalates. A colonic epithelial cell model was used to evaluate the effects of these phthalates at the concentrations found in water from plastic bottles. In cells exposed to phthalates, the increased expression of factors, which control the signaling pathways necessary for intestinal epithelium homeostasis, inflammatory response, and stress was detected. The proposed method falls fully within the limits imposed by the guidelines with precision (RSD%) below 7.1% and accuracy (BIAS%) within −4.2 and +6.1. Full article
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11 pages, 652 KiB  
Article
Influence of the Drying Method on the Volatile Component Profile of Hypericum perforatum Herb: A HS-SPME-GC/MS Study
by Karolina Dudek, Marcelin Jan Pietryja, Slawomir Kurkiewicz, Małgorzata Kurkiewicz, Barbara Błońska-Fajfrowska, Sławomir Wilczyński and Anna Dzierżęga-Lęcznar
Processes 2022, 10(12), 2593; https://doi.org/10.3390/pr10122593 - 05 Dec 2022
Cited by 1 | Viewed by 1321
Abstract
Hypericum perforatum L. (St. John’s wort) is one of the most popular medicinal plants in the world. Due to its documented antimicrobial and antioxidant properties, it is used in the treatment of bacterial and viral infections as well as inflammations. It is also [...] Read more.
Hypericum perforatum L. (St. John’s wort) is one of the most popular medicinal plants in the world. Due to its documented antimicrobial and antioxidant properties, it is used in the treatment of bacterial and viral infections as well as inflammations. It is also used to treat gastrointestinal diseases and mild to moderate depression. In recent years, there has been an increase in the popularity of herbal medicine. Many people collect their own herbs and dry them at home. A common choice for quick drying of fruits, vegetables and herbs at home are food dehydrator machines. There are not many publications in the scientific literature examining the quality of dried herbal material obtained in such dryers. We characterized St. John’s wort harvested in southern Poland and investigated the effect of specific drying methods on the volatile component profile. The herbal raw material was dried using three methods: indoors at room temperature, in an incubator at 37 °C and in a food dehydrator machine. Volatile components were analysed by HS-SPME GC/MS. The herb dried in a food dehydrator, compared to other drying methods, retained similar or slightly smaller amounts of the compounds from the mono- and sesquiterpenes group, aromatic monoterpenes, aromatic monoterpenoids, sesquiterpenoids, aromatic sesquiterpenes and alkanes. However, monoterpenoids and compounds coming from decomposition reactions, such as alcohols, short-chain fatty acids and esters, were noticed in larger quantities. Usage of a food dehydrator at home can be a convenient alternative to drying herbs. However, due to a different profile of volatile components depending on the drying method, the amount of biologically active substances needs to be considered. By using various methods of drying, the medical effects of herbs can be enhanced or weakened; therefore, further research in this direction should be continued. Full article
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15 pages, 3853 KiB  
Article
A New Approach for Increasing Speed, Loading Capacity, Resolution, and Scalability of Preparative Size-Exclusion Chromatography of Proteins
by Yating Xu, Si Pan and Raja Ghosh
Processes 2022, 10(12), 2566; https://doi.org/10.3390/pr10122566 - 02 Dec 2022
Cited by 1 | Viewed by 1952
Abstract
Low speed, low capacity, and poor scalability make size-exclusion chromatography (SEC) unattractive for use in the preparative separation of proteins. We discuss a novel z2 cuboid SEC device that addresses these challenges. A z2 cuboid SEC device (~24 mL volume) was [...] Read more.
Low speed, low capacity, and poor scalability make size-exclusion chromatography (SEC) unattractive for use in the preparative separation of proteins. We discuss a novel z2 cuboid SEC device that addresses these challenges. A z2 cuboid SEC device (~24 mL volume) was systematically compared with a conventional SEC column having the same volume and packed with the same resin. The primary objective of this study was to use the same volume of SEC medium in a much more efficient way by using the novel device. At any given flow rate, the pressure drop across the z2 cuboid SEC device was lower by a factor of 6 to 8 due to its shorter bed height and greater cross-sectional area. Under overloaded conditions, the peaks obtained during protein separation with the conventional column were poorly resolved and showed significant fronting, while those obtained with the z2 cuboid SEC device were much better resolved and showed no fronting. At any given flow rate, better resolution was obtained with the z2 cuboid SEC device, while for obtaining a comparable resolution, the flow rate that could be used with the z2 cuboid SEC device was higher by a factor of 2 to 3. Hence, productivity in SEC could easily be increased by 200 to 300% using the z2 cuboid SEC device. The scalability of the z2 cuboid SEC device was also demonstrated based on a device with a 200 mL bed volume. Full article
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9 pages, 1288 KiB  
Article
Are Plants Capable of Pheomelanin Synthesis? Gas Chromatography/Tandem Mass Spectrometry Characterization of Thermally Degraded Melanin Isolated from Echinacea purpurea
by Slawomir Kurkiewicz, Łukasz Marek, Małgorzata Kurkiewicz, Adam Kurkiewicz and Anna Dzierżęga-Lęcznar
Processes 2022, 10(11), 2465; https://doi.org/10.3390/pr10112465 - 21 Nov 2022
Cited by 2 | Viewed by 1516
Abstract
Echinacea is a widely used plant medicine, valued especially for its well-documented ability to stimulate the immune system. It has been suggested that melanin could be one of the bioactive factors responsible for the immunostimulatory properties of the plant. The biological functions of [...] Read more.
Echinacea is a widely used plant medicine, valued especially for its well-documented ability to stimulate the immune system. It has been suggested that melanin could be one of the bioactive factors responsible for the immunostimulatory properties of the plant. The biological functions of melanin pigments are closely related to their chemical composition and structural features. The aim of this study was to characterize the melanin from Echinacea purpurea based on the analysis of thermal degradation products of the well-purified pigment extracted from the dried herb. The melanin was pyrolyzed, and the resulting products were separated by gas chromatography and identified using a triple quadrupole mass spectrometer operating in full scan and multiple reaction monitoring modes. Three groups of marker products were detected in the melanin pyrolysate: polyphenol derivatives, nitrogen-containing heterocycles devoid of sulfur, and benzothiazines/benzothiazoles. This suggests that E. purpurea produces three structurally different melanin pigments: allomelanin, eumelanin, and pheomelanin, which in turn may affect the biological activity of the herb. Our results provide the first-ever evidence that plants are capable of synthesizing pheomelanin, which until now, has only been described for representatives of the animal and fungal kingdoms. Full article
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19 pages, 3204 KiB  
Article
Influence of Chromatographic Conditions on LOD and LOQ of Fluoxetine and Sertraline Analyzed by TLC-Densitometric Method
by Wioletta Parys and Alina Pyka-Pająk
Processes 2022, 10(5), 971; https://doi.org/10.3390/pr10050971 - 12 May 2022
Cited by 4 | Viewed by 1845
Abstract
This research introduces the analysis of fluoxetine and sertraline by means of the TLC-densitometric method. They provide information on LOD and LOQ under various chromatographic conditions. The study used adsorption (NPTLC) and partition (RPTLC) thin-layer chromatography in combination with a densitometric analysis. Four [...] Read more.
This research introduces the analysis of fluoxetine and sertraline by means of the TLC-densitometric method. They provide information on LOD and LOQ under various chromatographic conditions. The study used adsorption (NPTLC) and partition (RPTLC) thin-layer chromatography in combination with a densitometric analysis. Four types of chromatographic plates precoated with: silica gel 60 F254, silica gel 60, silanized silica gel 60 F254 (RP-2), and a mixture of silica gel 60 and kieselguhr F254, as well as three mobile phases: chloroform + methanol + ammonia (9:1:0.4, v/v/v), chloroform + methanol + glacial acetic acid (5:4:1, v/v/v), and acetone + toluene + ammonia (10:9:1, v/v/v), were used in NPTLC. RP-18F254 and silanized silica gel 60 F254 (RP-2) plates and four mobile phases: methanol + water (10:0 and 9:1, v/v), acetone + water (10:0 and 9:1, v/v), were used in RPTLC. The lowest LOD and LOQ values for fluoxetine were obtained using a silanized silica gel 60 F254 (RP-2) with acetone + toluene + ammonia (10:9:1, v/v/v) in NPTLC, and with a silanized silica gel 60 F254 (RP-2) in combination with methanol + water (10:0, v/v) in RPTLC. The lowest LOD and LOQ values of sertraline were obtained using a silica gel 60 with acetone + toluene + ammonia (10:9:1; v/v/v) in NPTLC. The smallest amount of sertraline was detected on the silanized silica gel 60 F254 plate in combination with methanol + water (9:1, v/v) in RPTLC. The obtained results provide important information that can give a good basis and set the direction for further, more detailed research; the results can also benefit other researchers who analyze fluoxetine and sertraline with the TLC technique in model systems (testing standards) as well as in drug and biological samples. Full article
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12 pages, 2153 KiB  
Article
Comparison of Two Extraction Procedures, SPE and DLLME, for Determining Plasticizer Residues in Hot Drinks at Vending Machines
by Ivan Notardonato, Sergio Passarella, Alessia Iannone, Cristina Di Fiore, Mario Vincenzo Russo, Carmela Protano, Matteo Vitali and Pasquale Avino
Processes 2021, 9(9), 1588; https://doi.org/10.3390/pr9091588 - 05 Sep 2021
Cited by 7 | Viewed by 2463
Abstract
This paper would like to compare two extraction procedures for analyzing phthalates (PAEs) in hot drinks collected at vending machines, usually coffee and tea. The two analytical procedures are based on Solid Phase Extraction (SPE) using C18 cartridge and on dispersive liquid-liquid microextraction [...] Read more.
This paper would like to compare two extraction procedures for analyzing phthalates (PAEs) in hot drinks collected at vending machines, usually coffee and tea. The two analytical procedures are based on Solid Phase Extraction (SPE) using C18 cartridge and on dispersive liquid-liquid microextraction (DLLME) assisted by ultrasound and vortex for improving the dispersion mechanically, with each followed by a routinary analytical method such as GC-FID. Seven phthalates (DMP, DEP, DiBP, DBP, DEHP, DOP, DDP) have been analyzed and determined. All the analytical parameters (i.e., recovery, limit of detection, limit of quantification, enrichment factors, repeatability, reproducibility) have been investigated and discussed, as has the matrix effect. The entire procedure has been applied to hot drink matrices, e.g., coffee, decaffeinated coffee, barley coffee, ginseng coffee and tea. Full article
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9 pages, 1030 KiB  
Article
Interaction between Antifungal Isoxazolo[3,4-b]Pyridin 3(1H)-One Derivatives and Human Serum Proteins Analyzed with Biomimetic Chromatography and QSAR Approach
by Krzesimir Ciura, Joanna Fedorowicz, Hanna Kapica, Monika Pastewska, Wiesław Sawicki and Jarosław Sączewski
Processes 2021, 9(3), 512; https://doi.org/10.3390/pr9030512 - 12 Mar 2021
Cited by 7 | Viewed by 1525
Abstract
The development of effective, nontoxic antifungal agents is one of the most important challenges for medicinal chemistry. A series of isoxazolo [3,4-b]pyridine-3(1H)-one derivatives previously synthesized in our laboratory demonstrated promising antifungal properties. The main goal of this study was [...] Read more.
The development of effective, nontoxic antifungal agents is one of the most important challenges for medicinal chemistry. A series of isoxazolo [3,4-b]pyridine-3(1H)-one derivatives previously synthesized in our laboratory demonstrated promising antifungal properties. The main goal of this study was to investigate their retention behavior in a human serum proteins-high-performance liquid chromatography (HSA-HPLC) system and explore the molecular mechanism of HSA-isoxazolone interactions using a quantitative structure–retention relationship (QSRR) approach. In order to realize this goal, multiple linear regression (MLR) modeling has been performed. The proposed QSRR models presented correlation between experimentally determined lipophilicity and computational theoretical molecular descriptors derived from Dragon 7.0 (Talete, Milan, Italy) software on the affinity of isoxazolones to HSA. The calculated plasma protein binding (PreADMET software) as well as chromatographic lipophilicity (logkw) and phospholipophilicity (CHIIAM) parameters were statistically evaluated in relation to the determined experimental HAS affinities (logkHSA). The proposed model met the Tropsha et al. criteria R2 > 0.6 and Q2 > 0.5 These results indicate that the obtained model can be useful in the prediction of an affinity to HSA for isoxazolone derivatives and they can be considered as an attractive alternative to HSA-HPLC experiments. Full article
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17 pages, 6573 KiB  
Article
LC-UV and UPLC-MS/MS Methods for Analytical Study on Degradation of Three Antihistaminic Drugs, Ketotifen, Epinastine and Emedastine: Percentage Degradation, Degradation Kinetics and Degradation Pathways at Different pH
by Anna Gumieniczek, Izabela Kozak, Paweł Żmudzki and Urszula Hubicka
Processes 2021, 9(1), 64; https://doi.org/10.3390/pr9010064 - 30 Dec 2020
Cited by 2 | Viewed by 2834
Abstract
Evaluation of pH-dependent reactivity of drugs is an essential component in the pharmaceutical industry. Thus, the stability of three antihistaminic drugs, i.e., ketotifen, epinastine and emedastine, was tested, in solutions of five pH values, i.e., 1.0, 3.0, 7.0, 10.0 and 13.0, at high [...] Read more.
Evaluation of pH-dependent reactivity of drugs is an essential component in the pharmaceutical industry. Thus, the stability of three antihistaminic drugs, i.e., ketotifen, epinastine and emedastine, was tested, in solutions of five pH values, i.e., 1.0, 3.0, 7.0, 10.0 and 13.0, at high temperature (70 °C). LC-UV isocratic methods were developed to estimate percentage degradation as well as the kinetics of degradation. Generally, epinastine was shown to be the most stable compound with degradation below 14%. Emedastine was labile in all pH conditions, with degradation in the range 29.26–51.88%. Ketotifen was moderately stable at pH 1–7 (degradation ≤ 14.04%). However, at pH ≥ 10, its degradation exceeded 30%. The kinetics of degradation of ketotifen, epinastine and emedastine was shown as a pseudo-first-order reaction with the rate constants in the range 10−4–10−3 min−1 Finally, the UPLC-MS/MS method was applied to identify the main degradants and suggest degradation pathways. Degradation of ketotifen proceeded with oxidation and demethylation in the piperidine ring of the molecule. As far as epinastine was concerned, opening of the imidazole ring with formation of the amide group was observed. Unfortunately, no degradation products for emedastine were detected. The present results complete the literary data and may be important for both manufacturing of these drugs and their administration to patients. Full article
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11 pages, 2085 KiB  
Article
A Comparative Study of Ethanol Concentration in Costal Cartilage in Relation to Blood and Urine
by Marcin Tomsia, Joanna Nowicka, Rafał Skowronek, Magdalena Woś, Joanna Wójcik, Kornelia Droździok, Magdalena Zorychta, Gulnaz T Javan and Elżbieta Chełmecka
Processes 2020, 8(12), 1637; https://doi.org/10.3390/pr8121637 - 11 Dec 2020
Cited by 6 | Viewed by 2972
Abstract
Blood is not always available in forensic autopsies, therefore, the search for alternative sampling materials is needed. This study aimed at examining if ethanol can be detected in costal cartilage and to investigate if different forms of costal cartilage can give accurate information [...] Read more.
Blood is not always available in forensic autopsies, therefore, the search for alternative sampling materials is needed. This study aimed at examining if ethanol can be detected in costal cartilage and to investigate if different forms of costal cartilage can give accurate information about ethanol concentration in the blood or urine of human cadavers (n = 50). Ethanol concentration in samples of unground costal cartilage (UCC), ground costal cartilage (GCC), femoral venous blood, and urine was analyzed using a gas chromatography-flame ionization detector (GC-FID). Due to Polish law, we used two different cut-off points: the blood alcohol concentration >0.2 mg/mL defined as the ‘after use’ condition, and the blood alcohol concentration >0.5 mg/mL defined as the ‘state of insobriety’. Based on the constructed receiver operating characteristics (ROC) curves, the optimal cut-off point for ethanol content as the ‘after use’ condition was 0.273 mg/g for the UCC method and 0.069 mg/g for the GCC method. Analysis of the Areas under a ROC Curve (AUC) showed that both methods present excellent diagnostic accuracy (AUCUCC = 0.903; AUCGCC = 0.984). We demonstrated that it is possible to detect ethanol in the costal cartilage and showed that ethanol concentrations are determined in GCC samples with greater accuracy. Full article
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13 pages, 831 KiB  
Article
Determination of Vitamins K1, K2 MK-4, MK-7, MK-9 and D3 in Pharmaceutical Products and Dietary Supplements by TLC-Densitometry
by Urszula Hubicka, Agnieszka Padiasek, Barbara Żuromska-Witek and Marek Szlósarczyk
Processes 2020, 8(7), 870; https://doi.org/10.3390/pr8070870 - 18 Jul 2020
Cited by 7 | Viewed by 7844
Abstract
Vitamin K is a group of lipophilic molecules. Forms of vitamin K play an essential role in the activation of specific proteins involved in blood clotting cascade or bone metabolism. Another molecule belonging to the fat-soluble vitamins group that also plays an important [...] Read more.
Vitamin K is a group of lipophilic molecules. Forms of vitamin K play an essential role in the activation of specific proteins involved in blood clotting cascade or bone metabolism. Another molecule belonging to the fat-soluble vitamins group that also plays an important role in calcium metabolism is vitamin D3. The dietary supplements containing vitamins K and D3 are one of the most frequently consumed by patients. The objective of this work was to develop a simple, fast and sensitive thin-layer chromatography (TLC)-densitometric procedure for the simultaneous quantitative analysis of vitamins K and D3 in pharmaceutical products and dietary supplements. The analysis of vitamins was performed on the silica gel RP-18 F₂₅₄s plates with methanol-ethanol-isopropanol in a volume ratio of 15:1:4 as a mobile phase. The densitometric measurements were made at 254 nm. The method was validated by checking the specificity, linearity, precision, recovery, limit of detection, limit of quantification and robustness in accordance with International Conference on Harmonization (ICH) guidelines. The method was shown to be specific, accurate (recoveries were from 95.78 to 104.96%), linear over the tested range (correlation coefficient, exceeding 0.99), and precise (precision and intermediate precision RSD below 2.70% for all analytes). The satisfactory results of the validation of the method indicate that it can be used in the quality control of dietary supplements and pharmaceutical products containing vitamins K and D3. Full article
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11 pages, 1195 KiB  
Article
Evaluation of the Lipophilicity of New Anticancer 1,2,3-Triazole-Dipyridothiazine Hybrids Using RP TLC and Different Computational Methods
by Beata Morak-Młodawska, Krystian Pluta and Małgorzata Jeleń
Processes 2020, 8(7), 858; https://doi.org/10.3390/pr8070858 - 17 Jul 2020
Cited by 12 | Viewed by 3433
Abstract
Two new anticancer-active 1,2,3-triazole-dipyridothiazine hybrids were evaluated for their lipophilicity using thin-layer chromatography (TLC) and computational methods. The experimental lipophilicity was evaluated with mobile phases (mixtures of TRIS buffer and acetone), exploiting a linear correlation between the retention parameter (RM) [...] Read more.
Two new anticancer-active 1,2,3-triazole-dipyridothiazine hybrids were evaluated for their lipophilicity using thin-layer chromatography (TLC) and computational methods. The experimental lipophilicity was evaluated with mobile phases (mixtures of TRIS buffer and acetone), exploiting a linear correlation between the retention parameter (RM) and the volume of acetone. The relative lipophilicity parameter (RM0) was obtained by extrapolation to 0% acetone concentration. This parameter was intercorrelated with a specific hydrophobic surface area (b) revealing two congeneric subgroups: hybrids of 1,2,3-triazole-2,7-diazaphenothiazines and 1,2,3-triazole-3,6-diazaphenothiazines. The parameter RM0 was converted into the absolute lipophilicity parameter logPTLC using a calibration curve prepared on the basis of compounds of known logP values. Triazole–dipyridothiazine hybrids turned out to be medium lipophilic with logPTLC values of 1.232–2.979. The chromatographically established parameter logPTLC was compared to the calculated lipophilic parameter logPcalcd obtained with various algorithms. The lipophilicity was correlated with molecular descriptors and ADME properties. The new triazole–dipyridothiazine hybrids followed Lipinski’s rule of five. The lipophilicity of these hybrids was dependent on the substituents attached to the triazole ring and the location of the azine nitrogen atoms. Full article
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12 pages, 1055 KiB  
Article
A Green RP-HPTLC-Densitometry Method for the Determination of Diosmin in Pharmaceutical Formulations
by Ahmed I. Foudah, Prawez Alam, Md. Khalid Anwer, Hasan S. Yusufoglu, Maged S. Abdel-Kader and Faiyaz Shakeel
Processes 2020, 8(7), 817; https://doi.org/10.3390/pr8070817 - 11 Jul 2020
Cited by 17 | Viewed by 3380
Abstract
Green analytical technologies for the determination of a bioactive compound diosmin (DIOM) in the real samples of pharmaceutical formulations and biological fluids are scarce in literature. Therefore, the present investigation was carried out to develop a novel, rapid, simple, and economical green “reversed [...] Read more.
Green analytical technologies for the determination of a bioactive compound diosmin (DIOM) in the real samples of pharmaceutical formulations and biological fluids are scarce in literature. Therefore, the present investigation was carried out to develop a novel, rapid, simple, and economical green “reversed phase high-performance thin-layer chromatography (RP-HPTLC)” method for the determination of DIOM in commercial tablets and in-house developed spray-dried microparticles (MPs). The quantification of DIOM was conducted via “RP-18 silica gel 60 F254S HPTLC plates”. The binary combination of green solvents, i.e., ethanol:water (5.5:4.5 v/v) was proposed as a green mobile phase. The analysis of DIOM was conducted in absorbance/reflectance mode of densitometry at λmax = 348 nm. The densitograms of DIOM from the commercial tablets and in-house developed spray-dried MPs were verified by recording their single band at Rf = 0.80 ± 0.02 compared to standard DIOM. Green RP-HPTLC method was observed as linear in the range of 100–700 ng/band with R2 = 0.9995. The proposed method was found as “accurate, precise, robust, and sensitive” for the determination of DIOM in the real samples of commercial tablets and in-house developed spray-dried MPs. The % content of DIOM in the real samples of commercial tablets and in-house developed spray-dried MPs was obtained as 99.06 and 101.30%, respectively. The recorded results of this research suggested that the green RP-HPTLC method can be effectively used for the routine analysis of DIOM in pharmaceutical products. Full article
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15 pages, 1232 KiB  
Article
TLC-Densitometric Determination of Five Coxibs in Pharmaceutical Preparations
by Paweł Gumułka, Monika Dąbrowska and Małgorzata Starek
Processes 2020, 8(5), 620; https://doi.org/10.3390/pr8050620 - 22 May 2020
Cited by 6 | Viewed by 4206
Abstract
A class of drugs called coxibs (COX-2 inhibitors) were created to help relieve pain and inflammation of osteoarthritis and rheumatoid arthritis with the lowest amount of side effects possible. The presented paper describes a new developed, optimized and validated thin layer chromatographic (TLC)-densitometric [...] Read more.
A class of drugs called coxibs (COX-2 inhibitors) were created to help relieve pain and inflammation of osteoarthritis and rheumatoid arthritis with the lowest amount of side effects possible. The presented paper describes a new developed, optimized and validated thin layer chromatographic (TLC)-densitometric procedure for the simultaneous assay of five coxibs: celecoxib, etoricoxib, firecoxib, rofecoxib and cimicoxib. Chromatographic separation was conducted on HPTLC F254 silica gel chromatographic plates as a stationary phase using chloroform–acetone–toluene (12:5:2, v/v/v) as a mobile phase. Densitometric detection was carried out at two wavelengths of 254 and 290 nm. The method was tested according to ICH guidelines for linearity, recovery and specificity. The presented method was linear in a wide range of concentrations for all analyzed compounds, with correlation coefficients greater than 0.99. The method is specific, precise (%RSD < 1) and accurate (more than 95%, %RSD < 2). Low-cost, simple and rapid, it can be used in laboratories for drug monitoring and quality control. Full article
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11 pages, 1870 KiB  
Article
Response Surface Methodology as a Useful Tool for Evaluation of the Recovery of the Fluoroquinolones from Plasma—The Study on Applicability of Box-Behnken Design, Central Composite Design and Doehlert Design
by Andrzej Czyrski and Hubert Jarzębski
Processes 2020, 8(4), 473; https://doi.org/10.3390/pr8040473 - 17 Apr 2020
Cited by 24 | Viewed by 5786
Abstract
The aim of this study was to find the best design that is suitable for optimizing the recovery of the representatives of the 2nd, 3rd and 4th generation of fluoroquinolones. The following designs were applied: Central Composite Design, Box–Behnken Design and Doehlert Design. [...] Read more.
The aim of this study was to find the best design that is suitable for optimizing the recovery of the representatives of the 2nd, 3rd and 4th generation of fluoroquinolones. The following designs were applied: Central Composite Design, Box–Behnken Design and Doehlert Design. The recovery, which was a dependent variable, was estimated for liquid–liquid extraction. The time of shaking, pH, and the volume of the extracting agent (dichloromethane) were the independent variables. All results underwent the statistical analysis (ANOVA), which indicated Central Composite Design as the best model for evaluation of the recovery. For each analyte, an equation was generated that enabled to estimate the theoretical value for the applied conditions. The graphs for these equations were provided by the Response Surface Methodology. The statistical analysis also estimated the most significant factors that have an impact on the liquid–liquid extraction, which occurred to be pH for ciprofloxacin and moxifloxacin and the volume of an extracting solvent for levofloxacin. Full article
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Review

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16 pages, 2647 KiB  
Review
Microbial Natural Products with Wound-Healing Properties
by Prima F. Hillman, Chaeyoung Lee and Sang-Jip Nam
Processes 2023, 11(1), 30; https://doi.org/10.3390/pr11010030 - 23 Dec 2022
Cited by 1 | Viewed by 2140
Abstract
Wound healing continues to pose a challenge in clinical settings. Moreover, wound management must be performed properly and efficiently. Acute wound healing involves multiple cell divisions, a new extracellular matrix, and the process of formation, such as growth factors and cytokines, which are [...] Read more.
Wound healing continues to pose a challenge in clinical settings. Moreover, wound management must be performed properly and efficiently. Acute wound healing involves multiple cell divisions, a new extracellular matrix, and the process of formation, such as growth factors and cytokines, which are released at the site of the wound to regulate the process. Any changes that disrupt the healing process could cause tissue damage and prolong the healing process. Various factors, such as microbial infection, oxidation, and inflammation, can delay wound healing. In order to counter these problems, utilizing natural products with wound-healing effects has been reported to promote this process. Several natural products have been associated with wound healing, most of which are from medicinal plants. However, secondary microbial metabolites have not been extensively studied for their wound-healing properties. Further, investigations on the wound-healing control of natural microbial products are required due to a lack of studies. This review discussed the in vivo and in vitro research on the wound healing activities of natural microbial products, which may assist in the development of better wound treatments in the future. Full article
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38 pages, 454 KiB  
Review
Significance of Chromatographic Techniques in Pharmaceutical Analysis
by Wioletta Parys, Małgorzata Dołowy and Alina Pyka-Pająk
Processes 2022, 10(1), 172; https://doi.org/10.3390/pr10010172 - 17 Jan 2022
Cited by 7 | Viewed by 7943
Abstract
This work presents an overview of the modern approaches embracing advanced equipment and validation parameters of both liquid and gas chromatography techniques, including thin-layer chromatography (TLC), column liquid chromatography (CLC), and gas chromatography (GC), suitable for the identification and quantitative determination of various [...] Read more.
This work presents an overview of the modern approaches embracing advanced equipment and validation parameters of both liquid and gas chromatography techniques, including thin-layer chromatography (TLC), column liquid chromatography (CLC), and gas chromatography (GC), suitable for the identification and quantitative determination of various bioactive compounds occurring in pharmaceutical products and medicinal plants in the time from 2020 to 2021 (November). This review confirmed that HPLC is an incredibly universal tool, especially when combined with different detectors, such as UV-Visible spectroscopy, mass spectrometry (MS), and fluorescence detection for numerous active ingredients in different pharmaceutical formulations without interferences from other excipients. TLC, in combination with densitometry, is a very efficient tool for the determination of biologically active substances present in pharmaceutical preparations. In addition, TLC coupled to densitometry and mass spectrometry could be suitable for preliminary screening and determination of the biological activity (e.g., antioxidant properties, thin layer chromatography (TLC) by 2,2-diphenyl-1-picrylhydrazyl (DPPH) method) of plant materials. Gas chromatography, coupled with a mass spectrometer (GC-MS, GC-MS/MS), is of particular importance in the testing of any volatile substances, such as essential oils. LC, coupled to NMR and MS, is the best solution for identifying and studying the structure of unknown components from plant extracts, as well as degradation products (DPs). Thanks to size-exclusion chromatography, coupled to multi-angle light scattering, the quality control of biological pharmaceuticals is possible. Full article
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