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Open AccessArticle

Development of a Zeolite H-ZSM-5-Based D-μSPE Method for the Determination of Organophosphorus Pesticides in Tea Beverages

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Processes 2023, 11(4), 1027; https://doi.org/10.3390/pr11041027 - 28 Mar 2023

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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

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Open AccessArticle

Development and Optimization of Chromatographic Conditions for the Determination of Selected B Vitamins in Pharmaceutical Products

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Joanna Żandarek

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Żaneta Binert-Kusztal

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Małgorzata Starek

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Monika Dąbrowska

Processes 2023, 11(3), 937; https://doi.org/10.3390/pr11030937 - 19 Mar 2023

Cited by 1 | Viewed by 726

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

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Open AccessFeature PaperArticle

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

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Processes 2023, 11(1), 45; https://doi.org/10.3390/pr11010045 - 25 Dec 2022

Viewed by 860

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

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Open AccessFeature PaperArticle

Influence of the Drying Method on the Volatile Component Profile of Hypericum perforatum Herb: A HS-SPME-GC/MS Study

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Karolina Dudek

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Marcelin Jan Pietryja

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Slawomir Kurkiewicz

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Małgorzata Kurkiewicz

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Barbara Błońska-Fajfrowska

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Sławomir Wilczyński

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Anna Dzierżęga-Lęcznar

Processes 2022, 10(12), 2593; https://doi.org/10.3390/pr10122593 - 05 Dec 2022

Viewed by 669

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

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Open AccessFeature PaperArticle

A New Approach for Increasing Speed, Loading Capacity, Resolution, and Scalability of Preparative Size-Exclusion Chromatography of Proteins

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Yating Xu

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Si Pan

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Raja Ghosh

Processes 2022, 10(12), 2566; https://doi.org/10.3390/pr10122566 - 02 Dec 2022

Viewed by 991

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

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Open AccessArticle

Are Plants Capable of Pheomelanin Synthesis? Gas Chromatography/Tandem Mass Spectrometry Characterization of Thermally Degraded Melanin Isolated from Echinacea purpurea

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Slawomir Kurkiewicz

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Łukasz Marek

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Małgorzata Kurkiewicz

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Adam Kurkiewicz

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Anna Dzierżęga-Lęcznar

Processes 2022, 10(11), 2465; https://doi.org/10.3390/pr10112465 - 21 Nov 2022

Cited by 1 | Viewed by 868

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

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Open AccessFeature PaperArticle

Influence of Chromatographic Conditions on LOD and LOQ of Fluoxetine and Sertraline Analyzed by TLC-Densitometric Method

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Wioletta Parys

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Alina Pyka-Pająk

Processes 2022, 10(5), 971; https://doi.org/10.3390/pr10050971 - 12 May 2022

Cited by 1 | Viewed by 1045

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

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Open AccessFeature PaperEditor’s ChoiceArticle

Comparison of Two Extraction Procedures, SPE and DLLME, for Determining Plasticizer Residues in Hot Drinks at Vending Machines

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Processes 2021, 9(9), 1588; https://doi.org/10.3390/pr9091588 - 05 Sep 2021

Cited by 3 | Viewed by 1761

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

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Open AccessArticle

Interaction between Antifungal Isoxazolo[3,4-b]Pyridin 3(1H)-One Derivatives and Human Serum Proteins Analyzed with Biomimetic Chromatography and QSAR Approach

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Processes 2021, 9(3), 512; https://doi.org/10.3390/pr9030512 - 12 Mar 2021

Cited by 6 | Viewed by 1086

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 (logk_w) and phospholipophilicity (CHI_IAM) parameters were statistically evaluated in relation to the determined experimental HAS affinities (logk_HSA). 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

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Open AccessFeature PaperArticle

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

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Processes 2021, 9(1), 64; https://doi.org/10.3390/pr9010064 - 30 Dec 2020

Cited by 1 | Viewed by 1840

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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

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Open AccessArticle

A Comparative Study of Ethanol Concentration in Costal Cartilage in Relation to Blood and Urine

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Processes 2020, 8(12), 1637; https://doi.org/10.3390/pr8121637 - 11 Dec 2020

Cited by 5 | Viewed by 2236

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 (AUC_UCC = 0.903; AUC_GCC = 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

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Open AccessFeature PaperArticle

Rapid TLC with Densitometry for Evaluation of Naproxen Stability

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Wioletta Parys

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Małgorzata Dołowy

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Alina Pyka-Pająk

Processes 2020, 8(8), 962; https://doi.org/10.3390/pr8080962 - 10 Aug 2020

Cited by 2 | Viewed by 2744

Abstract

The purpose of the work was to develop such chromatographic conditions that allowed to separate as many naproxen degradation products as possible. In order to follow this process, thin-layer chromatography (TLC) coupled with densitometry and spectrodensitometry was used. A forced degradation study was [...] Read more.

The purpose of the work was to develop such chromatographic conditions that allowed to separate as many naproxen degradation products as possible. In order to follow this process, thin-layer chromatography (TLC) coupled with densitometry and spectrodensitometry was used. A forced degradation study was performed using an ethanolic solution of naproxen spotted on silica gel plates, existing in the form of an aqueous solution at various pH values, and as solution prepared in saline and in hydrogen peroxide. Degradative effect of UV light on naproxen was watched in the context of naproxen spotted on plates precoated with silica gel and exposed to UV light, and also for its solution treated with UV light. However, the solution of naproxen prepared in water at pH ≈ 2.60 undergoes the largest changes as the results of its exposure to UV light during 10 h. Stressed samples of naproxen were analyzed by using a new and well validated TLC procedure including toluene (TOL)—acetone (ACE)—chloroform (CHL) (2:5:12, v/v/v) as mobile phase A and glacial acetic acid (AcOH)—n-hexane (Hex)—acetone (ACE)-(0.10:10:10, v/v/v) as mobile phase B. As the newly developed TLC-densitometric method can effectively separate the substances about pharmaceutical significance from products of its degradation, which are formed as a result of stress studies, is considered to be a good alternative and important tool in routine quality control and stability testing of naproxen in pharmaceutical formulations. These results indicate that proposed TLC-densitometric method is cost-effective, rapid, specific, accurate, and precise. This TLC procedure is comparable to HPLC and UPLC method in terms of detection the number of degradation products of naproxen. In addition, it realizes the criterion of linearity. A major advantage and novelty of proposed method is its low cost and ability to analyze examined drug and all degradation products simultaneously, including those which can be observed under intensive UV radiation exposure of naproxen solution which are not described by previous HPTLC studies available in the literature. Full article

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Open AccessFeature PaperArticle

Estimating Limits of Detection and Quantification of Ibuprofen by TLC-Densitometry at Different Chromatographic Conditions

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Josef Jampilek

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Malgorzata Dolowy

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Alina Pyka-Pajak

Processes 2020, 8(8), 919; https://doi.org/10.3390/pr8080919 - 02 Aug 2020

Cited by 8 | Viewed by 2808

Abstract

Ibuprofen is one of the best-known nonsteroidal anti-inflammatory and analgesic drugs. Following the previous work, the current study is focused on estimating the effect of different chromatographic conditions on the sensitivity of thin-layer chromatography in combination with UV densitometry, i.e., the detection and [...] Read more.

Ibuprofen is one of the best-known nonsteroidal anti-inflammatory and analgesic drugs. Following the previous work, the current study is focused on estimating the effect of different chromatographic conditions on the sensitivity of thin-layer chromatography in combination with UV densitometry, i.e., the detection and quantification of ibuprofen in a wide range of its concentrations including the lowest limits of detection (LOD) and quantification (LOQ). For this purpose, a reliable and easy-to-use calculation procedure for LOD and LOQ determination is presented in this work. In addition, the impact of type plates and mobile phase composition on the LOD and LOQ, respectively, of this active substance is accurately described. The results of detection and the quantification level of ibuprofen obtained under applied chromatographic conditions confirmed the utility of silica gel plates as well as silica gel bonded phases (i.e., reversed-phase (RP) plates) in the thin-layer chromatography (TLC)-densitometric analysis of ibuprofen at a low level, i.e., from several nanograms (below one microgram) to a few micrograms/spot. Among all chromatographic systems tested, the best are those consisting of silica gel 60F₂₅₄ plates with concentrating zone (1.05583) and the mixture of n-hexane:ethyl acetate:glacial acetic acid in ratio 36:12:2 (v/v/v) as well as RP plates, i.e., RP-18F₂₅₄ aluminum plates developed with methanol:water in volume composition 40:10 (v/v). These chromatographic systems allowed quantifying ibuprofen in the amount of 0.229 µg/spot and 0.228 µg/spot, which is less than 1 µg/spot. It can be stated that different chromatographic systems in combination with UV densitometric scanning at 224 nm proposed in this work can be successfully applied for the cost-effective and sensitive determination of ibuprofen as a widely used drug component as well as a residual in domestic wastewater. It was found that the modification of silica gel as well as the layer thickness of unmodified or modified silica gel 60 can influence the quality of chromatograms and the detection/quantification of ibuprofen in both normal phase (NP) and RP systems. Therefore, to obtain the best possible LOD and LOQ values of ibuprofen with precoated layers, suitable mobile phase and chromatographic plates are required. Full article

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Open AccessFeature PaperArticle

Determination of Vitamins K_1, K₂ MK-4, MK-7, MK-9 and D₃ in Pharmaceutical Products and Dietary Supplements by TLC-Densitometry

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Urszula Hubicka

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Agnieszka Padiasek

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Barbara Żuromska-Witek

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Marek Szlósarczyk

Processes 2020, 8(7), 870; https://doi.org/10.3390/pr8070870 - 18 Jul 2020

Cited by 4 | Viewed by 5360

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

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Open AccessFeature PaperArticle

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 11 | Viewed by 2568

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 (R_M) [...] 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 (R_M) and the volume of acetone. The relative lipophilicity parameter (R_M0) 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 R_M0 was converted into the absolute lipophilicity parameter logP_TLC using a calibration curve prepared on the basis of compounds of known logP values. Triazole–dipyridothiazine hybrids turned out to be medium lipophilic with logP_TLC values of 1.232–2.979. The chromatographically established parameter logP_TLC was compared to the calculated lipophilic parameter logP_calcd 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

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Open AccessArticle

A Green RP-HPTLC-Densitometry Method for the Determination of Diosmin in Pharmaceutical Formulations

by

,

,

,

,

and

Processes 2020, 8(7), 817; https://doi.org/10.3390/pr8070817 - 11 Jul 2020

Cited by 15 | Viewed by 2582

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 λ_max = 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 R_f = 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

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Open AccessFeature PaperEditor’s ChoiceArticle

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 2 | Viewed by 3384

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

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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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 18 | Viewed by 4365

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

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Review

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Open AccessReview

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

Viewed by 1002

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

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Open AccessFeature PaperReview

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 5 | Viewed by 3924

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

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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Open AccessFeature PaperReview

Current Strategies for Studying the Natural and Synthetic Bioactive Compounds in Food by Chromatographic Separation Techniques

by

Wioletta Parys

,

Małgorzata Dołowy

and

Alina Pyka-Pająk

Processes 2021, 9(7), 1100; https://doi.org/10.3390/pr9071100 - 24 Jun 2021

Cited by 1 | Viewed by 1484

Abstract

The present study summarizes the new strategies including advanced equipment and validation parameters of liquid and gas chromatography methods i.e., thin-layer chromatography (TLC), column liquid chromatography (CLC), and gas chromatography (GC) suitable for the identification and quantitative determination of different natural and synthetic [...] Read more.

The present study summarizes the new strategies including advanced equipment and validation parameters of liquid and gas chromatography methods i.e., thin-layer chromatography (TLC), column liquid chromatography (CLC), and gas chromatography (GC) suitable for the identification and quantitative determination of different natural and synthetic bioactive compounds present in food and food products, which play an important role in human health, within the period of 2019–2021 (January). Full characteristic of some of these procedures with their validation parameters is discussed in this work. The present review confirms the vital role of HPLC methodology in combination with different detection modes i.e., HPLC-UV, HPLC-DAD, HPLC-MS, and HPLC-MS/MS for the determination of natural and synthetic bioactive molecules for different purposes i.e., to characterize the chemical composition of food as well as in the multi-residue analysis of pesticides, NSAIDs, antibiotics, steroids, and others in food and food products. Full article

(This article belongs to the Special Issue Applications of Chromatographic Separation Techniques in Food and Chemistry)

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