液相色谱-串联质谱法测定尿样中11种苯二氮卓类药物及其代谢产物  

Simultaneous determination of benzodiazepines and their metabolites in urine by liquid chromatography-tandem mass spectrometry

作　　者：张建丽[1] 王占良[1] 张亦农[1] 

机构地区：[1]国家体育总局反兴奋剂中心,北京100029

出　　处：《分析试验室》2014年第4期479-482,共4页Chinese Journal of Analysis Laboratory

摘　　要：建立了同时检测尿样中11种苯二氮卓类药物及其代谢产物的液相色谱-串联质谱方法。尿样在pH 6.86磷酸盐缓冲液中经葡萄糖醛酸苷酶酶解后，在碱性条件下，用乙酸乙酯提取，以10mmoVL的甲酸铵（pH3．5）和乙腈为流动相，采用Agilent Zorbax SB C18（100mm×2.1mm，3.5 μm）色谱柱进行梯度分离，电喷雾离子源，正离子多反应监测扫描方式进行分析检测。结果表明：11种苯二氮卓类药物及其代谢产物在尿样中的检测限均不高于0.5ng／mL，在1.0～100.0ng／mL范围内线性关系良好，相关系数均大于0.9990。在低（1.0ng／mL）、中（10.0ng／mL）、高（100.0 ng／mL）3个浓度的提取回收率均在89.0％以上，相对标准偏差均不高于15％。方法适用于尿样中11种该类药物的定性定量测定。A simultaneous determination method for 11 benzodiazepines and their metabolites in urine by liquid chromatography-tandem mass spectrometry was established in this paper. Ethyl acetate was used as the extraction solution under alkaline condition after enzymolysis at pH 6. 86 with phosphate buffer. Mobile phase was 10 mmol/L ammonium formate （ pH 3.5 ） and acetonitrile. An Agilent Zorbax SB Cls （ 100 mm × 2.1 mm, 3.5 μm）column was used to separate the compounds with gradient elution and mass data were acquired with the positive electrospray ionization in the multiple reaction monitoring （MRM） mode. The limits of detection （LODs） of 11 benzodiazepines and their metabolites in urine were no more than 0.5 ng/mL. Good linearities were obtained between peak area ratio and concentrations in the range of 1.0 - 100. 0 ng/mL and correlation coefficients were above 0. 9990. The average recoveries of 11 target compounds with the concentration of low （1.0 ng/mL）, middle （10. 0 ng/mL） and high（ 100. 0 ng/mL） exceeded 89.0%, and the relative standard deviations （RSDs） were no more than 15%. This method was suitable for the qualitative and quantitative analysis of 11 benzodiazepines and their metabolites in urine.

关 键 词：苯二氮卓类药物 代谢产物 尿样 液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学]