SPE-GC-MS法检测尿液中丁丙诺啡及去环丙甲基丁丙诺啡

建立以氘代化合物为内标测定尿液中丁丙诺啡及去环丙甲基丁丙诺啡的GC-MS分析方法。尿液经β-葡萄糖醛酸酶水解后,加入d4-丁丙诺啡和d3-去环丙甲基丁丙诺啡氘代同位素内标物,固相萃取,经硅烷化试剂衍生化后,进行GC-MS-SIM模式分析。结果显示,在0.05～4.0μg/ml浓度范围内丁丙诺啡及去环丙甲基丁丙诺啡都呈现良好线性关系,相关系数分别为0.9997、0.9998,检出限分别为0.0017μg/ml,0.0085μg/ml;空白样品加标平均回收率86%,RSD分别为1.5%,2.3%。该方法简单、可靠、重复性好,可以应用于丁丙诺啡滥用者的尿液检测。

Determination of Buprenorphine and Norbuprenor-phine in Urine by SPE-GC-MS

Buprenorphine and norbuprenophine in urine were analyzed by gas chromatography-mass spectrometry using deuterated as internal standard.After the β-glucuronidase hydrolysis,d3-norbuprenophine and d4-buprenorphine were added into the urine samples.Then they were extracted by solid-phase extraction.The N,O-bis（trimethylsily） trifluoroacetamide was added to the extracts to derivative buprenorphine,norbuprenophine and the internal standards.The derivated analytes were determined by gas chromatographymass SIM mode.This method showed a high linearity from 0.05μg/ml to 4.0 μg/ml with correlation coefficients being 0.9997 and 0.9998.The limits of detection were 0.0017 μg/ml and 0.0085 μg/ml for the buprenorphine and norbuprenophine.And the recoveries of buprenorphine and norbuprenophine were more than 86% and the relative standard deviations（RSD） were 1.5% and 2.3%.This method is simple,reliable,reproducible,and can be applied to the detection of buprenorphine in the urine.