The optimization of the reversed-phase high-performance liquid chromatographic separation of a mixture of ethynylestradiol, desogestrel and three related compounds is described. A procedure is used that allows the prediction of the capacity factors of each individual synthetic steroid, depending on the mobile phase composition. Therefore, complete chromatograms can be predicted and evaluated with the multi-criteria decision making method.
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http://dx.doi.org/10.1016/s0021-9673(00)90030-x | DOI Listing |
J Chromatogr B Analyt Technol Biomed Life Sci
January 2025
Université Clermont Auvergne, Institut Universitaire de Technologie, UMR INSERM-UCA, U1240, Imagerie Moléculaire et Stratégies Théranostiques (IMoST), 5 Avenue Blaise Pascal, 63000 Clermont-Ferrand, France.
A method using high-performance liquid chromatography coupled with fluorescence detection (HPLC-FLD) was developed and validated to quantify the innovative tool LightSpot®-FL-1, a selective permeability-glycoprotein (P-gp)-targeted fluorescent conjugate used to measure P-gp expression in cell samples. Quantifying P-gp is a major challenge in oncology as its overexpression in many cancer cells results in Multidrug Resistance (MDR) associated with chemotherapy failure. To develop the method reported herein, both sample preparation and analysis parameters were investigated.
View Article and Find Full Text PDFPolymers (Basel)
January 2025
Engineering Research Center of Oil and Gas Field Chemistry, Universities of Shaanxi Provence, Xi'an Shiyou University, Xi'an 710065, China.
In order to solve the problems of long dissolution and preparation time, cumbersome preparation, and easy moisture absorption and deterioration during storage or transportation, acrylamide (AM), acrylic acid (AA), sodium p-styrene sulfonate (SSS), and cetyl dimethylallyl ammonium chloride (DMAAC-16) were selected as raw materials, and the emulsion thickener P(AM/AA/SSS), which can be instantly dissolved in water and rapidly thickened, was prepared by the reversed-phase emulsion polymerization method. DMAAC-16, the influence of emulsifier dosage, oil-water ratio, monomer molar ratio, monomer dosage, aqueous pH, initiator dosage, reaction temperature, reaction time, and other factors on the experiment was explored by a single-factor experiment, and the optimal process was determined as follows: the oil-water volume ratio was 0.4, the emulsifier dosage was 7% of the oil phase mass, the initiator dosage was 0.
View Article and Find Full Text PDFJ Proteome Res
January 2025
Corelabs, King Abdullah University of Science and Technology, Thuwal 23500-6900, Kingdom of Saudi Arabia.
We introduce here a novel approach, termed time-segmented acquisition (Seg), to enhance the identification of peptides and proteins in trapped ion mobility spectrometry (TIMS)-time-of-flight (TOF) mass spectrometry. Our method exploits the positive correlation between ion mobility values and reversed-phase liquid chromatography (LC) retention time to improve ion separation and resolution. By dividing the LC retention time into multiple segments and applying a segment-specific narrower ion mobility range within the TIMS tunnel, we achieved better separation and higher resolution of ion mobility.
View Article and Find Full Text PDFAnal Chim Acta
February 2025
Department of Analytical Chemistry, Faculty of Chemistry, Universitat de València, C/ Dr. Moliner 50, 46100, Burjassot, Spain. Electronic address:
Background: Developing analytical methods for Traditional Medicine products by liquid chromatography is challenging due to their chemical complexity and the lack of analytical standards for numerous, unidentified constituents. Regulatory agencies recommend chromatographic fingerprint analysis for quality evaluation, relying on peak detection to ensure resolution. Conventional modelling struggles to optimise experimental conditions for such complex samples.
View Article and Find Full Text PDFJ Chromatogr Sci
January 2025
Nutrition and Bromatology Group, Department of Analytical Chemistry and Food Science, Faculty of Science, Universidade de Vigo, E-32004 Ourense, Spain.
An efficient reverse-phase high-performance liquid chromatographic method, based on the design of the experiment approach, was developed for the simultaneous determination of capsiate isomers. Critical method parameters, i.e.
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