超高效液相色谱串联质谱法同时快速检验全血中扎来普隆及其代谢产物  

Determination of Zaleplon and Its Metabolites in Human Blood by QuEChERS-Ultra Performance Liquid Chromatography-Mass Spectrometry

作　　者：徐多麒 张蕾萍[2] 王继芬[1] 黄健[2] 郭震[1] 林宽[1] 

机构地区：[1]中国人民公安大学刑事科学技术学院,北京100038 [2]公安部物证鉴定中心,北京100038

出　　处：《分析化学》2016年第7期1059-1064,共6页Chinese Journal of Analytical Chemistry

基　　金：公安部重点研究计划项目(No.201302ZDYJ002);公安技术交流培训计划项目(No.B2014004A);2015年北京市教委科学研究与研究生共建项目资助

摘　　要：建立了全血中扎来普隆及其代谢产物5-氧扎来普隆和脱乙基扎来普隆超高效液相色谱-三重四级杆质谱(UPLC-TQ/MS)快速检验方法。采用改良后的QuEChERS前处理方法,全血样品用0.1%甲酸-乙腈提取,经无水MgSO_4脱水净化,Waters BEHC_(18)色谱柱分离,0.1%甲酸和0.1%甲酸-乙腈进行梯度洗脱。采用电喷雾电离,正离子(ESI+)模式扫描,多反应监测(MRM)模式检测。扎来普隆及其代谢产物在0.5~100 ng/mL范围内线性关系良好(R^2≥0.997),回收率为92.0%~100.1%,相对标准偏差为1.9%~5.3%,方法检出限(S/N=3)均为0.05 ng/mL,定量限(S/N=10)在0.1~0.5 ng/mL范围内。A fast testing method was established for the determination of zaleplon and its two metabolites, 5- oxozaleplon and desethylzaleplon, in blood by ultra performance liquid chromatography tandem eleetrospray ionization triple quadrapole-mass spectrometry （UPLC-TQ/MS）. The optimized QuEChERS （Quick, Easy, Cheap, Effective, Rugged and Safe ） method was used for sample preparation. The blood samples were extracted with 0.1% acetic acid and dehydrated by adding anhydrous magnesium sulfate. The targets were separated on a Waters BEH C18 column by gradient elution with 0. 1% formic acid-0. 1% formic acid/ acetonitrile as mobile phase, ionized with positive electrospray （ESI^＋）, and detected under multiple reaction monitoring （MRM） mode. As a result, zaleplon and its two metabolites displayed excellent linearity in the concentration of 0.5-100 ng/mL （R^2〉0. 997）. The average recoveries ranged from 92.0% to 100.1%. The RSD were in the range of 1.9%-5.3%. Besides, the limit of detection（LOD）of this method for target drugs was 0.05 ng/mL （ S/N = 3 ）, while limits of quantification （ LOQ ） were in the range of 0.1-0.5 ng/mL （S/N= 10） . This method can meet the demand of rapidity and accuracy in the analysis of actual cases.

关 键 词：扎来普隆 5-氧扎来普隆 脱乙基扎来普隆 QuEChERS方法 超高效液相色谱串联质谱法 

分 类 号：O657.63[理学—分析化学] D918.93[理学—化学]