肿瘤药学2019，Vol.9Issue(3)：500-504,514,6.DOI:10.3969/j.issn.2095-1264.2019.03.31
基于LC-MS技术测定人血浆中吉西他滨浓度方法学的建立与临床应用★
Establishment and Application of the Method for Determination of Gemcitabine Concentration in Human Plasma by Liquid Chromatography / Tandem Mass Spectrometry★
摘要
Abstract
Objective To establish a method for the determination of gemcitabine concentration in human plasma by liquid chromatography-tandem mass spectrometry (LC-MS). Methods The sample plasma 200 μL was precipitated protein by adding acetonitrile. After 30 s vortex, the plasma was centrifuged at 9000 rpm for 5 min. The supernatant was filtered and 0.22 μm was taken to determine. The Agilent ZORBAX Eclipse Plus C18 (2.1×150 mm 1.8-Micron) chromatographic column was adopted, and acetonitrile containing 0.1% formic acid and water containing 0.1% formic acid were used as mobile phase. Electrospray ionization (ESI) ion source mass spectrometry and multiple reaction monitoring (MRM) were used for positive ion detection. Results The calibration curve exhibited a linear dynamic range of 5~500 ng·mL-1. The detection limit of quantitative lower limit was 0.052 ng·mL-1. The linear equation was y=1272.93x+11213.5, r=0.999. The recovery rate of the three concentration levels (10, 50, 400 ng·mL-1) were respectively 93.41%, 98.22% and 96.95%, and the intraday relative standard deviation (RSD) were 4.55%, 3.09% and 2.81%, respectively. The RSD was 2.36%~4.78% after 24 h at room temperature and 2~4 ℃, 7.98%~11.67% after 90 days at -20℃, and 13.87%~16.52% after 180 days at -80 ℃. The concentration of gemcitabine in 24 human plasma samples was (13.84±5.61) μg·mL-1. Conclusion An accurate, simple and sensitive method for determining the plasma concentration of gemcitabine by LC-MS was available. It can be used in the determination of plasma concentration and pharmacokinetics of gemcitabine.关键词
吉西他滨/血药浓度/LC-MS/方法学/临床应用Key words
Gemcitabine/Blood concentration/LC-MS/Methodology/Clinical application分类
医药卫生引用本文复制引用
席加喜,张华君,陈晓宇,谢嫣嫣,龚倩..基于LC-MS技术测定人血浆中吉西他滨浓度方法学的建立与临床应用★[J].肿瘤药学,2019,9(3):500-504,514,6.基金项目
广西壮族自治区食品药品监督管理局2016年食品药品安全科研项目(区直自选0018) （区直自选0018）
广西壮族自治区卫生和计划生育委员会广西医药卫生自筹经费计划课题(z2016610). （z2016610）
