In this study, the chiral stationary phase was prepared by bonding vancomycin to 5 microm spherical silica gel according to "one-pot" synthetic strategies, and used to separate the enantiomers of zolmitriptan under polar ionic mode. The influences of mobile phase composition, such as the concentration and ratio of glacial acetic acid (HOAc) and triethylamine (TEA), on the enantioseparation were investigated, and the chiral recognition mechanism is discussed. It was found experimentally that the retention factors were increased with the increase of the HOAc/TEA concentration in a certain extent, and the ionic interactions, hydrogen bondings, and steric interactions may play key role together. The method is suitable for baseline separation of zolmitriptan enantiomers.
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http://dx.doi.org/10.1002/jssc.200500238 | DOI Listing |
Biomed Chromatogr
February 2025
Department of Pharmaceutical Chemistry and Analysis, ISF College of Pharmacy, Moga, Punjab, India.
Enantioseparation and enantiorecognition are crucial in the pharmaceutical analysis of chiral substances, impacting safety, efficacy, and regulatory compliance. Enantioseparation refers to the process of separating enantiomers from a mixture, typically achieved through chromatography techniques like HPLC and SFC. In contrast, enantiorecognition involves the identification of enantiomers based on their interaction with a chiral selector without the need for separation.
View Article and Find Full Text PDFOrg Chem Front
December 2024
Department of Chemistry, University of Basel St Johanns-Ring 19 Basel 4056 Switzerland https://www.chemie1.unibas.ch/Bmayor/.
This work explores the use of a cross-shaped organic framework that is used as a template for the investigation of multi-functionalized chromophores. We report the design and synthesis of a universal cross-shaped building block bearing two bromines and two iodines on its peripheral positions. The template can be synthesized on a gram scale in a five-step reaction comprising an oxidative homo-coupling macro-cyclization.
View Article and Find Full Text PDFJ Sep Sci
December 2024
College of Chemistry and Chemical Engineering, Yunnan Normal University, Kunming, China.
Chiral macrocycles have emerged as attractive media for chromatographic enantioseparation due to their excellent host-guest recognition properties. In this study, a new chiral stationary phase (CSP) based on 1,1'-binaphthyl chiral polyimine macrocycle (CPM) was reported. The CPM was synthesized by one-step aldehyde-amine condensation of (S)-2,2'-dihydroxy-[1,1'-binaphthalene]-3,3'-dicarboxaldehyde with 1,2-phenylenediamine and bonded on thiolated silica via the thiol-ene click reaction to afford the CSP.
View Article and Find Full Text PDFJ Chromatogr A
December 2024
I. U. CINQUIMA, Analytical Chemistry Group (TESEA), Dept. Analytical Chemistry, Faculty of Sciences, University of Valladolid 47011, Valladolid, Spain. Electronic address:
The simultaneous separation of the enantiomers of six anticoagulant rodenticides, derived from 4-hydroxycoumarin, has been studied in this work. Ten different stationary phases (zwitterionic, Pirkle-type, polysaccharides and macrocyclic antibiotics derivatives) were evaluated by using supercritical fluid chromatography coupled to two different detectors (circular dichroism and mass spectrometry-single quadrupole). The effect of the type of organic modifier and temperature on the chiral separation was investigated, and the best results were obtained with the column Regis S,S-Whelk-O1 at 25 °C when using a gradient elution program with methanol as organic modifier.
View Article and Find Full Text PDFJ Chromatogr B Analyt Technol Biomed Life Sci
December 2024
School of Ecology and Environment, Yuzhang Normal University, No.1999, Meiling Ave., Honggutan Dist., Nanchang 330103, Jiangxi, China.
Benzene, toluene, and xylene (BTX) are priority pollutants known for their hematotoxicity and carcinogenic properties. Benzene is further metabolized to phenyl mercapturic acid (PMA), toluene and xylene also generate benzyl mercapturic acid (BMA) in human urine. To confirm whether the exposure to benzene series comes from the workplace or from the external environment such as smoking is a very meaningful work, so accurate measurement of their biomarkers in biological samples is crucial.
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