title: Development and validation of an LC-MS/MS-ESI method for the determination of lorglumide, a CCK-1 antagonist in mouse plasma: application to a pharmacokinetic study.
abstract: A highly sensitive, rapid assay method was developed and validated for the estimation of lorglumide in mouse plasma using liquid chromatography coupled to tandem mass spectrometry with electrospray ionization in positive-ion mode. The assay procedure involves extraction of lorglumide and phenacetin (internal standard, IS) from mouse plasma with simple protein precipitation. Chromatographic separation was achieved using an isocratic mobile (0.2% formic acid solution-acetonitrile, 20:80, v/v) at a flow-rate of 0.5 mL/min on an Atlantis dC₁₈ column maintained at 40 °C with a total run time of 4.0 min. The MS/MS ion transitions monitored were 459.2 → 158.4 for lorglumide and 180.1 → 110.1 for IS. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. The lower limit of quantitation achieved was 0.42 ng/mL and the linearity range extended from 0.42 to 500 ng/mL. The intra- and inter-day precisions were in the ranges of 1.47-10.9 and 3.56-7.53, respectively.
authors: Drug Metabolism and Pharmacokinetics, Jubilant Biosys Ltd, Industrial Suburb, Yeshwanthpur, Bangalore 560022, India.
authors: Kuldeep
authors: K
authors: Sharma
authors: Anitha
authors: A
authors: Police
authors: Avinash
authors: A
authors: Kumar
authors: Gopal V
authors: GV
authors: Pawar
authors: Sanjeev
authors: S
authors: Giri
authors: Sriram
authors: S
authors: Rajagopal
authors: Ramesh
authors: R
authors: Mullangi
mesh_terms: D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006727:Hormone Antagonists / Q000097:blood / Q000493:pharmacokinetics; D016014:Linear Models; D008297:Male; D051379:Mice; D008810:Mice, Inbred C57BL; D010615:Phenacetin; D011377:Proglumide / Q000031:analogs & derivatives* / Q000097:blood / Q000493:pharmacokinetics; D011949:Receptors, Cholecystokinin / Q000037:antagonists & inhibitors; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods / Q000592:standards; D053719:Tandem Mass Spectrometry / Q000379:methods* / Q000592:standards
chemical_list: D006727:Hormone Antagonists; D011949:Receptors, Cholecystokinin; D011377:Proglumide; D010615:Phenacetin; C048181:lorglumide