Simultaneous enantioseparation with sensitive detection of four basic drugs, namely methoxamine, metaproterenol, terbutaline and carvedilol, using a 20-mum ID capillary with native beta-CD as the chiral selector was demonstrated by the large-volume sample stacking method. The procedure included conventional sample loading either hydrodynamically or electrokinetically at longer injection times without polarity switching and EOF manipulation. In comparison to conventional injections, depending on the analyte, about several hundred- and a thousand-fold sensitivity enhancement was achieved with the hydrodynamic and the electrokinetic injections, respectively. The simple method developed was applied to the analysis of racemic analytes in serum samples and better recovery was achieved using hydrodynamic injection than electrokinetic injection.
Download full-text PDF |
Source |
---|---|
http://dx.doi.org/10.1002/elps.200700299 | DOI Listing |
Anal Chim Acta
February 2025
Institute of Physical and Analytical Chemistry, School of Exact and Natural Sciences, Tbilisi State University, 0179, Tbilisi, Georgia. Electronic address:
Background: Isotopologues resulting from the labelling of molecules with deuterium have attracted interest due to the isotope effect observed in chemistry and biosciences. Isotope effect may also play out in noncovalent interactions and mechanisms leading to intermolecular recognition. In chromatography, differences in retention time between isotopologues, as well as between isotopomers have been observed resulting in two different elution sequences (isotope effects): the normal isotope effect when heavier isotopologues retain longer than lighter analogues, and the inverse isotope effect featuring the opposite elution order.
View Article and Find Full Text PDFFood Chem
February 2025
College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou 311121, China. Electronic address:
A novel, deep eutectic solvent (DES)-assisted sodium cholate (SC)-chiral microemulsion electrokinetic chromatography method is presented for separation of five flavonoid glycoside enantiomers, namely hesperidin, naringin, narirutin, eriocitrin, and neoeriocitrin. Herein, we develop a novel, green DES, whose addition considerably enhances the separation performance through multiple synergistic effects. A series of factors notably affecting chiral separation are systematically optimized: type and concentration of cyclodextrin, DES, and SC, oil phase type, and pH.
View Article and Find Full Text PDFJ Pharm Biomed Anal
September 2024
Institute of Physical and Analytical Chemistry, School of Exact and Natural Sciences, Tbilisi State University, 1 Ilia Chavchavadze Avenue, Tbilisi 0179, Georgia. Electronic address:
A method of analysis was developed for the simultaneous chemo- and enantioseparation of 2-, 3-, and 4-chloromethcathinones by high-performance liquid chromatography tandem mass-spectrometry. The fast method enables the reliable identification of positional isomers of chloromethcathinones in biological samples. In addition, the same method can be used for the enantioselective quantitative determination of one of these compounds and its major phase-1 metabolites in biological fluids.
View Article and Find Full Text PDFInt J Mol Sci
February 2024
Department of Pharmaceutical Chemistry, Semmelweis University, Hogyes 9, H-1092 Budapest, Hungary.
A reversed-phase high-performance liquid chromatographic (HPLC) method was developed for the simultaneous determination of the potential impurities of dexketoprofen, including the distomer R-ketoprofen. After screening the separation capability of four polysaccharide columns (Lux Amylose-1, Lux Amylose-2, Lux Cellulose-1 and Lux Cellulose-2) in polar organic and in reversed-phase modes, appropriate enantioseparation was observed only on the Lux Amylose-2 column in an acidified acetonitrile/water mixture. A detailed investigation of the mobile phase composition and temperature for enantio- and chemoselectivity showed many unexpected observations.
View Article and Find Full Text PDFChirality
March 2024
School of Chemical Sciences, University of Chinese Academy of Sciences, Beijing, China.
Given the markedly different pharmacological activities between enantiomeric isomers, it is crucial to encourage the stereoselective determination of chiral drugs in the biological and pharmaceutical fields, and the combination of drugs makes this analysis more complicated and challenging. Herein, a capillary electrophoresis (CE) method for the enantioseparation of ofloxacin and duloxetine was established, enabling the simultaneous identification of four isomers in nonracemic mixtures with enantiomeric excess (ee%) values exceeding 5%. This was achieved through the integration of theoretical simulation and electron circular dichroism (ECD), all without reliance on individual standards.
View Article and Find Full Text PDFEnter search terms and have AI summaries delivered each week - change queries or unsubscribe any time!