超高效液相色谱-串联质谱法检测中成药中添加格列本脲、格列吡嗪  

UPLC/MS/MS determination of glyburide and glipizide added in traditional Chinese medicinal preparation

作　　者：张翠英[1] 徐金玲[1] 李振国[1] 刘乃强[1] 

机构地区：[1]河南省食品药品检验所,郑州450003

出　　处：《药物分析杂志》2008年第2期326-328,共3页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立快速、准确、高灵敏度的检测中成药降糖制剂中非法添加格列本脲、格列吡嗪的分析方法。方法:采用 C_(18)(50 mm×2.1 mm,1.7 μm)柱分离,以乙腈-0.01 mol·L^(-1)乙酸铵(0.1%乙酸)缓冲溶液梯度洗脱,流速0.3 mL·min^(-1),以多反应检测(MRM)方式进行检测。用于定量分析的二级碎片离子分别为 m/z 321(格列吡嗪)和 m/z 369(格列本脲)。结果:格列吡嗪和格列本脲的线性范围分别为4.98～498 ng·mL^(-1)和4.96～496 ng·mL^(-1)。结论:此方法选择性强,灵敏度高,可作为中成药中非法添加格列本脲、格列吡嗪的分析检测方法。Objective ：To establish a UPLC/MS/MS method for analysis of glyburide and glipizide added in traditional Chinese medicinal preparation. Method： The mobile phase consisted of acetronitrile - ammonium acetate （0. 1% acetic acid） buffer,at a flow rate of 0.3 mL · min^-1. Electrospay ionization （ESI） source was applied and operated in the positive ion mode. The multiple reaction monitoring （MRM） mode use the transition of m/z 446→ 321 and m/z 494→369 were used to quantify the glipizide and glyburide, respectively. Results：The assay was linear from 4. 98 to 498 ng ~ mL -1 （glipizide） and from 4.96 to 496 ng · mL^-1 （glyburide）. Condusion： The method is selective and sensitive and can be used to detect and determine the contents of glyburide and glipizide illegally added into traditional Chinese medicinal preparations.

关 键 词：超高效液相色谱 串联质谱 多反应监测 格列本脲 格列吡嗪 

分 类 号：R917[医药卫生—药物分析学]