The coupling of capillary electrophoresis (CE) with capacitively coupled contactless conductivity detection (C D) has become convenient analytical method for determination of small molecules that do not possess chromogenic or fluorogenic group. The implementations of CE with C D in the determination of inorganic and organic ions and amino acids in biomedical field are demonstrated. Attention on background electrolyte composition, sample treatment procedures, and the utilize of multi-detection systems are described.
View Article and Find Full Text PDFThe study of antibody-antigen interactions, through epitope mapping, enhances our understanding of antibody neutralization and antigenic determinant recognition. Epitope mapping, employing monoclonal antibodies and mass spectrometry, has emerged as a rapid and precise method to investigate viral antigenic determinants. In this report, we propose an approach to improve the accuracy of epitopic peptide interaction rate recognition.
View Article and Find Full Text PDFChiral high performance liquid chromatographic technique usually employs polysaccharide-based stationary phases in a normal phase mode. This frequently generates large waste of organic solvents. Using shorter columns of 50 mm length as well as a mobile phase with a high water percentage are common approaches for greening this analytical technique.
View Article and Find Full Text PDFCoffee is a complex mixture of chemicals, which provide biologically active compounds with various health benefits. The some biologically active compounds arising from both its natural structure and formed after processing were determined as an antioxidant capacity of coffee beverages. In this study, we aimed to determine how roasting levels of Arabica coffee seed (light, medium, dark) and three brewing techniques-decoction methods (Turkish coffee), infusion method (filter coffee) and pressure methods (Espresso)-affect total antioxidant capacity in a cup of coffee beverage by electrochemical methods such as square wave stripping voltammetry (SWSV), differential pulse stripping voltammetry (DPSV) and cyclic voltammetry (CV).
View Article and Find Full Text PDFEnantioseparation of five β-adrenergic blockers was studied using two mobile phases on a cellulose tris(3-chloro-4-methylphenylcarbamate) (Lux-Cellulose-2) chiral column in normal phase mode. The first mobile phase composed of n-hexane: ethanol: diethylamine 60: 40: 0.1 by volume has successfully resolved the chromatographic peaks of three pairs of β-adrenergic blockers namely, bisoprolol, carvedilol and atenolol.
View Article and Find Full Text PDFComb Chem High Throughput Screen
October 2023
The recent development of monolithic chiral stationary phases (CSPs) for liquid chromatography (LC) is mainly focused on reducing backpressure, maximizing flow rates, faster run time, column efficiency, and stability. This review paper emphasizes recent progress in the development of polysaccharide and cyclodextrin-based monolithic CSPs. Further the paper draws attention to competing techniques, like non-porous particle-packed columns, core-shell and monoliths as chromatographic support matrix, available for achieving fast and efficient chromatographic separation.
View Article and Find Full Text PDFComb Chem High Throughput Screen
October 2023
2-Arylpropionic acid nonsteroidal anti-inflammatory drugs (NSAIDs) provide one of the most demonstrated pharmaceutical examples of chiral inversion. Chiral inversion depends on various factors (. biological-, solvent-, light-, temperature-induced, .
View Article and Find Full Text PDFA multimode sensor (a sensor responding simultaneously to more than one mode, e.g., stochastic mode, amperometric mode, voltammetric mode) based on graphite paste modified with -methylfulleropyrrolidine was proposed for the determination of butoconazole nitrate in its pharmaceutical formulation.
View Article and Find Full Text PDFThree chiral pyrazoline derivatives were synthesized by a flavanone ring-opening reaction followed by cyclocondensation with hydrazine hydrate to give better yields. Their enantiomeric resolution was achieved using polysaccharide chiral stationary phase columns consisting of cellulose (Chiralcel®OD-RH, Chiralcel®OZ-3) and amylose (Chiralpak®IA) by high-performance liquid chromatography. The separation was affected by the nature and concentration of the alcohol modifiers in the mobile phase.
View Article and Find Full Text PDFAnal Bioanal Chem
September 2022
Arginine has an important role in the metabolomics of gastric cancer. Two 3D enantioselective needle stochastic sensors based on the physical immobilization of 2,3,7,8,12,13,17,18-octaethyl-21H,23H-porphine manganese(III) chloride (solution, 10 mol L) in graphene paste matrices decorated with N and S atoms were designed, characterized and validated for the enantioanalysis of arginine in whole blood and tissue samples. The signature values obtained for the enantiomers of arginine confirmed that the stochastic sensors are enantioselective.
View Article and Find Full Text PDFThe sample preparation step is the initial step in pharmaceutical analysis. While ultrafiltration is a well-known technique used in the food and pharmaceutical industries, it has rarely been used to measure the plasma concentration of active pharmaceutical ingredients. This study aimed to analyze diclofenac sodium (DS) in human plasma samples using ultrafiltration-based sample preparation before high-performance liquid chromatography (HPLC) analysis.
View Article and Find Full Text PDFJ Chromatogr B Analyt Technol Biomed Life Sci
February 2022
Glutathione S-transferase P1 (GST-P1) is considered as a detoxification enzyme and can be upregulated in several cancers. Therefore, qualification and/or quantification of GST-P1 in biological fluids can be noteworthy in cancer diagnostic and/or prognostic methods. Whereas costly immunoassays methods are routinely used for clinical analysis, long analysis time per sample is still considered as their disadvantages.
View Article and Find Full Text PDFThe development of chiral selectors for the separation and analysis of chiral molecules has been an evolving process happening over three decades, since the introduction of the first chiral stationary phase (CSP) in 1938. The main impetus for designing new chiral selectors is to get to most promising one which has a broad chiral recognition property, separation capability for a wide range of chiral analytes, and the cost-effective CSP, which is also a major concern. Today, we have more than 100 commercially available CSPs, and these are prepared by coating or immobilizing the classical chiral selectors on to the chromatographic support, normally, silica gel.
View Article and Find Full Text PDFDespite organophosphorus pesticides (OPPs) benefits in controlling vector-borne diseases and noxious insects, the bioaccumulation and persistence in the soil system may metamorphose into new substances which could pose a serious threat to the ecosystems and human health. The generally low levels of OPPs residues and often the complexity of the soil matrix are the issues that researcher must deal with. Thus, it is essential to isolate and preconcentrate the OPPs from the matrix to reduce interference effects to obtain a reliable detection.
View Article and Find Full Text PDFJ Dent
September 2021
In this work, enantiomeric separation of a drug combination of two chiral drugs, namely, atenolol and chlorthalidone, is described. Prior investigation of the effect of different variables on the resolution of the enantiomers' peaks and the total run time represented by the retention time of the last eluted peak was conducted using face-centered composite design. Twenty-two experiments were carried out by varying the chiral stationary phase type as a categorical factor and mobile phase composition including the percentage of ethanol and percentage of diethylamine as continuous factors.
View Article and Find Full Text PDFSynthesis of three chiral 4,5-Di methyl ∆ N-phenyl N-aryl imidazole-2-thione derivatives was obtained by the condensation reaction of thiourea derivatives with α-hydroxy ketone. The structure of these compounds has been characterized by using spectroscopic methods (UV, IR, H NMR, and C NMR). The 4,5-Di methyl ∆ N-phenyl N-aryl imidazole-2-thiones display a chiral axis around the N-C bond linking between the nitrogen of the heterocyclic framework and the carbon of the aryl group.
View Article and Find Full Text PDFChiral molecules in relation to particular biological roles are stereoselective. Enantiomers differ significantly in their biochemical responses in biological environment. Despite the current advancement in drug discovery and pharmaceutical biotechnology, the chiral separation of some racemic mixtures continues to be one of the greatest challenges, because the available techniques are too costly and time consuming for the assessment of therapeutic drugs in the early stages of development worldwide.
View Article and Find Full Text PDFA thionation reaction was performed on some chiral flavanones using Lawesson's reagent (LR) and leads to the formation of new chiral thiocarbonyl flavanes. LR in this thionation reaction with Hesperetin and Naringenin gives new flavan-4-thiones with yields ranged between 41 and 52%. Based on the Wittig reaction principle, LR is currently the most widely used reagent for this type of reaction.
View Article and Find Full Text PDFRecent success in studying the proteome, as a source of biomarkers, has completely changed our understanding of leukemia (blood cancer). The identification of differentially expressed proteins, such as relapse and drug resistance proteins involved in leukemia by using various ionization sources and mass analyzers of mass spectrometry techniques, has helped scientists find better diagnosis, prognosis, and treatment strategies. With the aid of this powerful analytical technique, we can investigate the qualification/quantification of proteins, protein-protein interactions, post-translational modifications, and find the correlation between proteins and their genes with the hope of finding the missing parts of the successful therapy puzzle.
View Article and Find Full Text PDFA novel analytical method, based on high-performance liquid chromatography with a UV (HPLC-UV) detection system for the sensitive detection of a genotoxic impurity (GTI) 5-amino-2-chloropyridine (5A2Cl) in a model active pharmaceutical ingredient (API) tenoxicam (TNX), has been developed and validated. The HPLC-UV method was used for the determination of GTI 5A2Cl in API TNX. The compounds were separated using a mobile phase composed of water (pH 3 adjusted with orthophosphoric acid): MeOH, (50:50: v/v) on a C18 column (150 × 4.
View Article and Find Full Text PDFObjective: This paper analyzes the potential outliers in the bioanalytical and clinical part of a bioequivalence study, the effect on bioequivalence decisions whether or not it is appropriate to eliminate them from the statistical evaluation of bioequivalence.
Materials And Methods: The clinical part was a cross-over, two periods, two sequences bioequivalence study concerning two piroxicam formulations, on healthy subjects. A simulation study evaluated the influence of 10% errors on the percent bias of calculated concentrations from nominal ones.
Capacitively coupled contactless conductivity detection (CD) has emerged as influential to detect analytes that do not have chromogenic or fluorogenic functional group. Since our last review several new capillary electrophoresis (CE) methods coupled with (CE-CD) have been communicated. The aim of this review is to give an update of the almost all the new applications of CE-CD in the field of pharmaceutical, food and biomedical analysis covering the period from 2017 to April 2020.
View Article and Find Full Text PDFAdulteration of olive oil with the other cheap oils and fats plays an important role in economics and has nutritional benefits. In this work, metabolite profiling was performed using gas chromatography-mass spectrometry to identify and quantify animal fat (lard) adulteration in vegetable oil (olive oil). Principal component analysis could correctly identify and clustering olive oil, sunflower oil, sesame oil, lard, and adulterated samples through the changes in their fatty acid methyl esters (FAMEs) profile.
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