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A rapid and highly sensitive method for the determination of glimepiride in human plasma by liquid chromatography–electrospray ionization tandem mass spectrometry: application to a pre‐clinical pharmacokinetic study
Author(s) -
Chakradhar Lagishetty,
Kallem Rajareddy,
Karthik Arumugam,
Sundari Bala Tripura,
Ramesh Srirangam,
Mullangi Ramesh,
Srinivas Nuggehally R.
Publication year - 2008
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.896
Subject(s) - chromatography , chemistry , electrospray ionization , mass spectrometry , ammonium acetate , extraction (chemistry) , glimepiride , tandem mass spectrometry , liquid chromatography–mass spectrometry , electrospray , sample preparation , ethyl acetate , high performance liquid chromatography , medicine , type 2 diabetes , diabetes mellitus , endocrinology
A sensitive and specific liquid chromatography–positive electrospray ionization–tandem mass spectrometry method has been developed and validated for the determination of glimepiride (GPD) in human plasma. GPD and the internal standard (IS, glibenclamide) were extracted from a small aliquot of human plasma (200 µL) by a simple liquid–liquid extraction technique using ethyl acetate as extraction solvent. The compounds were separated on a YMC Propack, C 18 , 4.6 × 50 mm column using a mixture of ammonium acetate buffer, acetonitrile and methanol (30:60:10, v/v) as mobile phase at 0.5 mL/min on an API 4000 Sciex mass spectrometer connected to an Agilent HPLC system. Method validation and pre‐clinical sample analysis was performed as per FDA guidelines and the results met the acceptance criteria. GPD and IS were detected without any interference from human plasma matrix. The method was proved to be accurate and precise at linearity range of 0.02–100.00 ng/mL with a correlation coefficient of 0.999. The method was robust with a lower limit of quantitation of 0.02 ng/mL. Intra‐ and inter‐day accuracies for GPD were 88.60–113.50 and 96.82–103.93%, respectively. The inter‐day precision was better than 12.21%. This method enabled faster and reliable determination of GPD in a pre‐clinical study. Copyright © 2007 John Wiley & Sons, Ltd.