摘要
目的 建立LC-MS/MS法测定人血浆中厄洛替尼及其代谢产物去甲厄洛替尼的浓度.方法 血浆样品经甲醇沉淀蛋白后,以甲醇-水（含40 mmol/L NH4Ac）=70∶30（体积比）为流动相,采用ultimate XB-C18（4.6 mm×150 mm,5μm）色谱柱进行分离,流速为0.9 mL/min,通过电喷雾离子化串联质谱,以多反应监测（MRM）方式进行检测.结果 厄洛替尼线性范围为0.5～2 000 ng/mL（r=0.999 0）,去甲厄洛替尼线性范围为0.5～2 000 ng/mL（r=0.999 7）,最低定量下限均为0.5 ng/mL,厄洛替尼平均方法回收率为106.1％～ 108.7％,去甲厄洛替尼平均方法回收率为103.5％～ 105.5％,日内和日间变异均小于15％.结论 该方法具有快速简便、灵敏准确等特点,可满足厄洛替尼及其代谢物临床药物浓度测定的需要.
Objective To develop a liquid chromatography-tandem mass spectrometry method to determine erlotinib and its metabolites norerlotinib in human plasma. Methods After protein precipitation with methanol,erlotinib,norerlotinib and internal standard were separated on a C18 column（ ultimate,4.6 mm× 150 mm,5 μm） with a mobile phase containing methanol and water （40 mmol/L ammonium acetate buffer） = 70：30（Ф） at a flow rate of 0.9 mL/min.The electronic spray ion tandem mass spectrum with the positive mode and multitude reaction monitor （MRM） were used to detect the analytes.Results The linear range of the calibration curves was all 0.5-2 000 ng/mL for erlotinib and norerlotinib.The lower limit of quantification was all 0.5 ng/mL.Within-and between-run precision was was than 15%.The recovery ranged from 106.1%-108.7% for erlotinib and from 103.5%-105.5% for norerlotinib.Conclusion The method is sensitive, efficient and reliable which has been successfully used for the concentration assay of erlotinib and its metabolites norerlotinib.
出处
《广东药学院学报》
CAS
2014年第2期142-145,共4页
Academic Journal of Guangdong College of Pharmacy
基金
广东省科技计划项目(2010B031500031
2012B031800163)
广州市科技计划项目(2010YI-C931)
吴阶平临床科研基金(320.6700.09043)
