SPE-LC-MS/MS法同时测定尿液中氯氮平及三种代谢产物  

Determination of urine clozpzine and its three metobolites with SPE-LC-MS/MS

作　　者：谭晓辉[1] 尉志文[1] 于晓巍[1] 贠克明[1] 

机构地区：[1]山西医科大学法医学院,太原市030001

出　　处：《实用医学杂志》2013年第5期808-810,共3页The Journal of Practical Medicine

基　　金：十一五国家支撑计划项目(编号:2007BAK26B05)

摘　　要：目的:建立尿液中氯氮平(CPZ)、去甲氯氮平(DMCPZ)、N-氧氯氮平(N-OCPZ)和葡萄糖醛酸氯氮平(CPZ-G)的SPE-LC-MS/MS方法。方法:采用OASISHLB3cc(60mg)固相萃取柱进行提取,应用LC-MS/MS方法进行检测,运用保留时间和MRM方式对尿液中CPZ及其代谢物进行定性定量分析。结果:CPZ、DMCPZ、N-OCPZ、CPZ-G的回收率分别为91.55%～97.03%,96.95%～103.57%,85.31%～90.63%,85.02%～91.21%;最低检测限(LOD)依次为7.9、8.31、5.27、5.32pg,线性范围5～2000ng/mL;相关系数分别为0.9992、0.9958、0.9962、0.9974。结论:本研究所建方法,适用于尿液中CPZ及其主要代谢产物的提取净化与检测分析。Objective To establish a SPE-LC-MS/MS method for determination of clozpzine, DMCPZ, N- OCPZ, and CPZ-G in human urine. Methods Clozpzine and its three metobolites were extracted from human urine using OASIS HLB 3 ec （60 mg） extraction cartridges and then detected by LC-MS/MS. Retention time （Rt） and multiple reaction monitoring （MRM） were used to detect these compounds qualitatively and quantitatively. Results The recovery rate was 91.55% - 97.03% for clozpzine, 96.95% - 103.57% for DMCPZ, 85.31% - 90.63% for N-OCPZ, and 85.02%- 91.21% for CPZ-G. Limits of detection （LOD） was 7.9 pg, 8.31 pg, 5.27 pg, and 5.32 pg, respectively. The linear range was 5-2 000 ng/mL. The correlation coefficient of CPZ, DMCPZ, N- OCPZ, or CPZ-G was 0.999 2, 0.995 8, 0.996 2, and 0.997 4, respectively. Conclusions This method is suitable for extraction, purification, detection, and analysis of clozpzine and its major metabolites in human urine.

关 键 词：氯氮平 法医毒物分析 去甲氯氮平 N-氧氯氮平 葡萄糖醛酸氯氮平 尿液 

分 类 号：R96[医药卫生—药理学]