SPE-LC-MS/MS法测定尿液与血液中海洛因3种代谢物

目的采用SPE-LC-MS/MS方法,同时检测尿液与血液中海洛因主要代谢物3-β-D-葡萄糖醛酸吗啡(M3G)、吗啡和O6-单乙酰吗啡(O6)。方法采用BAKERBONDTMspe Octadecyl(C18)进行提取,应用LC-MS/MS方法检测并通过MRM及内标法进行量化。结果尿液中M3G、吗啡、O6-单乙酰吗啡的最低检测限(LOD)分别为1.24pg、6.71pg、0.47pg;回收率依次为82.25±12.25%、93.75±13.25%、88.70±11.90%。血液中M3G、吗啡、O6-单乙酰吗啡的最低检测限分别为1.50pg、8.21pg、0.52pg。回收率依次为89.85±21.15%、73.70±17.90%、90.10±3.90%。结论本文所建方法同时适用于尿液与血液中海洛因主要代谢物M3G、吗啡、O6-单乙酰吗啡的提取、净化、分析。

Determination of morphine3-glucuronide, morphine and O6-monoacetylmorphine in urine and plasma by LC-MS/MS with molid phase extraction

Objective To use the method which can accurately measure the metabolites of heroin(including morphine,morphine3-glucuronide and O6-Monoacetylmorphine) in urine and plasma by LC-MS/MS with solid-phase extraction.Methods the samples were extracted by BAKERBONDTM spe Octadecyl(C18) Disposable Extraction Columns 3cc 500mg and then detected by LC-MS-MS,quantification of compounds was achieved using multiple reactionmonitoring(MRM) incorporating the use of deuterated O6-Monoacetylmorphine as internal standards.Results Limits of Detection(LOD) were 1.24pg for M3G,6.71pg for morphine and 0.47pg for O6-Monoacetylmorphin in urine and 1.5pg for M3G,8.21pg for morphine and 0.52pg for O6-Monoacetylmorphin in plasma.In urine the recoveries for M3G,morphine,O6-Monoacetylmorphine were 82.25±12.25%、93.75±13.25%、88.70±11.90% respectively,and in plasma were 89.85±21.15%,73.70±17.90%,90.10±3.90%.Conclusion The method is suitable for extraction,purification and quantitative analysis of morphine,morphine3-glucuronide and O6-Monoacetylmorphine both in human urine and plasma.