Rapid and Specific Approach for Direct Measurement of Glimepiride in Human Plasma by LC-ESI-MS-MS Employing Automated 96 Well Format: Application to a Bioequivalence Study

Abstract

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.

Development and application of an analytical method for curdione quantification in pregnant sprague–dawley rats by LC‐MS/MS

“…1(C and D), the mass spectrometer was operated in electrospray ionization-positive ion mode, and ions were detected in the SRM mode by monitoring the transition of the m/z 237.2 precursor ion to the m/z 135.1 product ion for curdione and the transition of the m/z 491.3 precursor ion to the m/z 352.1 product ion for glimepiride. The target fragment ions were in good agreement with published references (Kundlik et al, 2012;Ma et al, 2012).…”

“…1A; Deng et al, 2006;Hikino et al, 1967;Hou et al, 2011;Jiang et al, 2010;Xia et al, 2012;Yan et al, 2005) Bansal et al, 2008;Kundlik et al, 2012) was the internal standard (IS) for the LC-MS/MS and was provided by Dr Reddy's Laboratories Ltd, India. The LC-MS/MS method was successfully applied for the toxicokinetic study of curdione by vaginal suppository administration to pregnant Sprague-Dawley rats.…”

“…The LC-MS/MS method was successfully applied for the toxicokinetic study of curdione by vaginal suppository administration to pregnant Sprague-Dawley rats. Deng et al, 2006;Hikino et al, 1967;Hou et al, 2011;Jiang et al, 2010;Xia et al, 2012;Yan et al, 2005) Bansal et al, 2008;Kundlik et al, 2012) was the internal standard (IS) for the LC-MS/MS and was provided by Dr Reddy's Laboratories Ltd, India. The methanol and acetonitrile (ACN) used in this study were HPLC grade and were purchased from DIKMA (Illinois, USA).…”

Rapid, Validated UPLC-MS/MS Method for Determination of Glibenclamide in Rat Plasma

“…In mass tuning, the method has different observation from prior art publications. While tuning, protonated glibenclamide and glimepiride molecules [M + H + ] were observed [ 6 , 18 , 19 ], but the signal intensity of their peaks were weak. The signal intensity of sodium ion [Na + ] adducts of glibenclamide as well as of glimepiride was significantly high than their protonated molecules [M + H + ].…”

The toxicokinetic profile of curdione in pregnant SD rats and its transference in a placental barrier system detected by LC–MS/MS

“…Glimepiride (C 24 H 34 N 4 O 5 S, purity 99.9%, Fig. 1) was the internal standard (IS) for the LC-MS/MS and was provided by Dr. Reddy's Laboratories Ltd. (Hyderabad, India) (Bansal et al, 2008;Kundlik et al, 2012). The methanol and acetonitrile (ACN) were HPLC-grade and were purchased from DIKMA (Illinois, USA).…”