Validated hydrophilic interaction LC-MS/MS method for determination of N-methyl-2-pyrrolidinone residue. Applied to a depletion study of N-methyl-2-pyrrolidinone in swine liver following intramuscular administration of drug N-methyl-2-pyrrolidinone formulation

文献类型: 外文期刊

第一作者: Liu, Yanhong

作者: Liu, Yanhong;Ji, Yanhong;Chen, Jingtao;Chen, Ximing;Wang, Guangxiang;Shang, Youjun;Liu, Xiangtao;Pan, Jack

作者机构:

关键词: N-methyl-2-pyrrolidinone;C18+WAX;LC-MS/MS;Matrix effect

期刊名称:JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES ( 影响因子:3.205; 五年影响因子:3.068 )

ISSN: 1570-0232

年卷期: 2010 年 878 卷 31 期

页码:

收录情况: SCI

摘要: A hydrophilic interaction high-performance liquid chromatography coupled with tandem mass spectrometry method for determination of N-methyl-2-pyrrolidinone in swine liver was developed and validated After the fortification of N-methyl-d(3)-2-pyrrolidinone-d(6) as the deuterium-labeled Internal standard N-methyl-2-pyrrolidinone in swine liver was extracted by acetonitrile and the supernatant was led through a C18 + WAX mixed-mode SPE cartridge for removal of the matrix interferences The final eluate was acidified by formic acid and then injected onto a 3 mu m 15 cm x 2 1 mm TX column for hydrophilic interaction chromatographic analysis Mass spectrometry detection was carried on a PE Sciex API 4000 triple quadrupole mass spectrometer using positive turbo-ion spray ionization mode The MRM transitions were 100 -> 58 for N-methyl-2-pyrrolidinone and 109 -> 62 for N-methyl-d(3)-2-pyrrolidinone-d(6) Solvent calibration standards could be readily used for quantitative analysis of N-methyl-2-pyrrolidinone with excellent precision and accuracy although there are endogenous levels of N-methyl-2-pyrrolidinone in many blank matrices The true recovery was nearly 100% and the MRM signal of N-methyl-2-pyrrolidinone was suppressed about 30% because of the matrix effect Nevertheless N-methyl-d(3)-2-pyrrolidinone-d(6) completely compensated the ion-suppression effect and the injection-to-injection variation The detection limit was 5 ng g(-1) swine liver The validated method was applied to a depletion study of N-methyl-2-pyrrolidinone in swine liver following intramuscular administration of a drug N-methyl-2-pyrrolidinone formulation (C) 2010 Elsevier B V All rights reserved

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