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黄克建,李宏森,朱定姬,林翠梧,李璐,刘晓锋.SPE-GC-MS法检测尿液中丁丙诺啡及去环丙甲基丁丙诺啡[J].广西科学院学报,2010,26(3):258-260,263. [点击复制]
- HUANG Ke-jian,LI Hong-sen,ZHU Ding-ji,LIN Cui-wu,LI Lu,LIU Xiao-feng.Determination of Buprenorphine and Norbuprenor-phine in Urine by SPE-GC-MS[J].Journal of Guangxi Academy of Sciences,2010,26(3):258-260,263. [点击复制]
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| SPE-GC-MS法检测尿液中丁丙诺啡及去环丙甲基丁丙诺啡 |
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黄克建1, 李宏森1, 朱定姬2, 林翠梧3, 李璐1, 刘晓锋1
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| (1.广西壮族自治区公安厅物证鉴定中心, 广西南宁 530012;2.广西职业病防治研究院, 广西南宁 530021;3.广西大学化学化工学院, 广西南宁 530004) |
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| 摘要: |
| 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0.05~4.0 μg/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0.0017 μg/ml,0.0085 μg/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。 |
| 关键词: 气相色谱-质谱联用法 固相萃取 丁丙诺啡 去环丙甲基丁丙诺啡 氘代内标 衍生化 |
| DOI： |
| 投稿时间：2010-04-02 |
| 基金项目:公安部应用创新计划项目(2007YYCXGXST081);广西壮族自治区公安厅科学研究与技术开发计划项目(桂公(科技)[2005]4号)资助。 |
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| Determination of Buprenorphine and Norbuprenor-phine in Urine by SPE-GC-MS |
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HUANG Ke-jian1, LI Hong-sen1, ZHU Ding-ji2, LIN Cui-wu3, LI Lu1, LIU Xiao-feng1
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| (1.Institution of Forensic Science, Public Security Department of Guangxi Zhuang Autonomous Region, Nanning, Guangxi, 530012, China;2.Guangxi Institute of Occupational Disease Prevention and Treatment, Nanning, Guangxi, 530021, China;3.College of Chemistry and Chemical Engineering, Guangxi University, Nanning, Guangxi, 530004, China) |
| Abstract: |
| 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 chromatography-mass 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. |
| Key words: gas chromatography-mass spectrometry solid phase extraction buprenorphine norbuprenorphine deuterated internal standard derivatization |
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