LC-MS/MS法测定人血浆中格列吡嗪的含量  

Determination of glipizide in human plasma by LC-MS/MS

作　　者：孙雪[1,2] 秦永平[3] 赵华[1] 

机构地区：[1]重庆医科大学药学院药物分析教研室,重庆400016 [2]西藏自治区人民医院药剂科,西藏850000 [3]四川大学华西医院临床药理研究室,四川成都610041

出　　处：《现代预防医学》2014年第17期3198-3200,共3页Modern Preventive Medicine

摘　　要：目的建立一种准确、灵敏的高效液相色谱串联质谱（LC-MS/MS）法测定格列吡嗪血药浓度。方法采用API3000型LC-MS/MS液质联用系统,Phenomenex C18分析柱（50 mm×3.0 mm,5μm）,流动相为甲醇︰水︰甲酸（62︰38︰0.025）,流速为0.2 ml/min,样品在酸性条件下用二氯甲烷提取浓集后进样,采用电喷雾离子源（ESI）,正离子MRM模式测定,卡马西平作为内标。结果检测格列吡嗪在1～1 000μg/L浓度范围内线性关系良好,定量限为1μg/L,批内和批间精密度分别小于4.47%和6.00%,方法回收率在89.86%～94.50%。结论本法具有快速简便、灵敏、准确等特点,适用于血浆中格列吡嗪含量测定及临床药代动力学研究。Objective To establish a sensitive and specific liquid chromatography tandem mass spectrometry（LC-MS/MS） method for determination of glipizide in human plasma. Methods The essay was conducted with an API 3000 LC-MS/MS system consisted of a Phenomenex C18column（50 mm×3.0 mm, 5 μm）; the mobile phase consisted of methanol-water-formic（62： 38： 0.025） in a flow rate of 0.2 ml·min^-1. The sample was extracted with dichloromethane under acidic conditions and was operated under the multiple reaction monitoring mode using the electrospray ionization technique.The carbamazepine was used as internal standard. Results The linear range of glipizide was 1-1 000 μg·L^-1. The limit of quantification was 1 μg·L^-1. Intraday and interday precision were below 4.47% and 6.00%, respectively. The method recoveries ranged from 89.86% to 94.50%. Conclusion This method is proved to be accurate, sensitive, convenient and suitable for determination of glipizide in human plasma and for clinical pharmacokinetic studies.

关 键 词：格列吡嗪 血浆药物浓度 LC-MS/MS 

分 类 号：R115[医药卫生—公共卫生与预防医学]