A Claisen-Schimidt condensation of 2-hydroxyacetophenones 1a-f with an aldehyde 2 yielded a series of compounds 3a-f. Compounds 3a-f were transformed into series of substituted chromones 4a-f, pyrazolines 5a-f and aurones 6a-f on treatment with DMSO/ I 2 , NH 2 NH 2 / EtOH and Hg(OAc) 2 / pyridine respectively. All these novel compounds were characterized by spectral techniques. All the compounds were screened for their antibacterial potential.
A rapid liquid chromatographic method with electrospray ionization tandem mass spectrometric (LC-MS-MS) detection is developed and validated for quantification of glimepiride in heparinized human plasma. Plasma samples, without a drying and reconstitution step, are extracted by solid-phase extraction (SPE) and eluted with 0.9 mL of acetonitrile-methanol (1:1, v/v) containing 0.05% formic acid. The analyte and glimepiride d8 (internal standard, IS) are chromatographed on a C(18) column; the mobile phase is acetonitrile-2 mm ammonium formate (88:12, v/v), with the pH adjusted to 3.5 with formic acid, at a flow rate of 0.5 mL/min. The retention times of glimepiride and the IS are 0.93 min, and the runtime is 1.6 min per sample. Selected reaction monitoring of MH(+) at m/z 491.20 and 499.26 result in stable fragment ions with m/z 351.80 and 359.96 for glimepiride and the IS, respectively. The response was a linear function of the concentration in the range of 2.0-650.0 ng/mL, with r ≥ 0.9994. The recovery of glimepiride and the IS ranged from 81.91 to 83.36%. The assay has excellent characteristics and has been successfully used for the analysis of glimepiride in healthy human subjects in a bioequivalence study. It was well suited to clinical studies of the drug involving large numbers of samples.
A rapid liquid chromatography coupled with ESI tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantification of topiramate in heparinized human plasma. The plasma samples were prepared by solid-phase extraction (SPE) method without drying and then reconstitution. Topiramate and the topiramate d-12 internal standard (IS) were chromatographed on a Betasil C18 column at a flow rate of 0.5 mL/min. The total run time was 1.80 min. An ESI interface with negative ion mode was selected for ionization of analyte and IS. The mass transition [M-H] ions used for detection were m/z 338.10→78.20 for topiramate, m/z 350.40→90.10 for IS. The method was linear in the concentration range of 10-4200 ng/mL with r≥0.9992. Recovery of topiramate and IS ranged from 78.20 to 87.74%. The validated method has been successfully used to analyze human plasma samples for application in 100 mg fasted and fed pharmacokinetic studies.
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