超高效液相色谱-串联质谱法检测血液斑痕中磺酰脲类降糖药  

Determination of three sulfonylureass in blood spot by ultra performance liquid chromatography-mass spectrometry

作　　者：杨煜[1] 张云峰[2] 李昕潼 王芳琳[2] 何洪源[1] 黄健[2] 

机构地区：[1]中国人民公安大学,北京100089 [2]公安部物证鉴定中心,北京100089

出　　处：《分析试验室》2017年第12期1390-1393,共4页Chinese Journal of Analysis Laboratory

基　　金：国家重点研发计划(2017YFC0803504);公安部技术研究计划(2015JSYJC49)项目资助

摘　　要：建立了血液斑痕中格列本脲,格列美脲,格列吡嗪的液相色谱-质谱检验法。选用ACQUITY UPLC HSS C18(2.1×50 mm,1.8μm)色谱柱,使用0.1%甲酸水-乙腈体系作为流动相进行梯度洗脱。采用ESI+电喷雾离子源,多反应监测扫描模式(MRM)检测3种磺酰脲类降糖药。在最优条件下,磺酰脲类降糖药在1.25~250 ng/patch(swab)范围内有良好线性关系,保留时间依次为2.90,3.00,2.34 min。检出限为0.1 ng/mL。渗透性客体上药物的回收率随着浓度的增大而增大,非渗透性客体上药物的回收率随着浓度的增大而减小。日内与日间精密度均小于15%,基质效应在0.85~1.15之间。可用于血液斑痕中格列本脲,格列美脲,格列吡嗪的快速筛查。A liquid chromatography-mass spectrometry （ LC - MS ） method for the determination of glibenclamide, glimepiride and glipizide in bloodstains was established. The ACQUITY UPLC HSS C18 （2.1 ×50 mm, 1.8μm） column was eluted using a 0.1% formic acid water-acetonitrile system as the mobile phase. The three sulfonylurea drugs were detected by LC-MS ESI ＋ electrospray ionization source mode and multi-reaction monitoring scanning mode （MRM）. Under the optimal conditions, the three sulfonylurea drugs had a good linearity in the range of 1.25 - 250 ng/patch （swab） with the retention time of 2.90, 3.00 and 2.34 min, respectively. The detection limits Were 0. 1 ng/mL. The recovery of the drug on the permeable guest increasedwith the increase of the concentration, and the recovery rateof the drug on the non - permeable guest decreased with the increase of the concentration. Day and day precisionswere less than 15% with the matrix effect between 0.85 1.15. This method can be used for rapid screening of glibenelamide, glimepiride, and glipizide in bloodstains.

关 键 词：磺酰脲类降糖药 血液斑痕 超高效液相色谱-串联质谱 

分 类 号：R917[医药卫生—药物分析学]