固相萃取／LC-MS／MS测定尿液中吗啡类药物

目的 建立尿液中吗啡类药物的固相萃取／LC—MS／MS方法。方法采用OASIS MCX3cc（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方式对尿液中吗啡类药物及其代谢物进行定性定量分析。结果磷酸盐缓冲液pH4．0时，海洛因、6-MAM、可待因、吗啡、M3G的固相萃取回收率分别达64．33％-70．21％，96．95％～117．57％，83．60％～123．63％，68．82％～91．03％，94．64％～107．33％；最低检测限（LOD）分别为5、10、5、5、2pg，线性范围0．005～10μg／mL；相关系数分别为0．9998、0．9958、0．9992、0．9994、0．9997。结论本文所建方法，适用于尿液中吗啡类药物的分析。

The determination of morphines in urine with LC-MS/MS by SPE

Objective To establish a solid phase extraction(SPE)/ LC-MS/MS method for determination of morphines in human urine.Methods Morphines were extracted from human urine using OASISMCX 3cc(60mg) extraction cartridges and detected by LC-MS/MS.Qualitative and quantitative analysis was obtained by retention time(Rt) and Multiple Reaction Monitoring(MRM) of LC-MS/MS.Results The recoveries for heroin,6-MAM,codeine,morphine,M3G were 64.33%~70.21%,96.95%~117.57%,83.60%~123.63%,68.82%~91.03%,94.64%~107.33% respectively,using phosphate buffer,pH4.0.Limits of Detection(LOD) were 5pg for M3G,10pg for morphine,5pg for codeine,5pg for 6-MAM and 2pg for heroin.The linear range is 0.005~10μg/mL.The correlation coefficient of heroin,6-MAM,codeine,morphine,M3G were 0.999 7,0.999 4,0.999 2,0.995 8,0.999 8 respectively.Conclusion The results of this study suggest that the method is simple,rapid and accurate for quantitative analysis of morphines and their metabolites in human urine.