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LC/MS分析血浆中丁丙诺啡
引用本文:刘冬娴,龚志平,陈本美. LC/MS分析血浆中丁丙诺啡[J]. 中国法医学杂志, 2010, 25(3): 172-174
作者姓名:刘冬娴  龚志平  陈本美
作者单位:1. 湖南公安高等专科学校刑事技术系,湖南,长沙,410138
2. 湖南省公安厅刑事科学技术研究所,湖南,长沙,410001
3. 中南大学分析测试中心,湖南,长沙,410078
基金项目:公安部科研项目公科研 
摘    要:目的建立血浆中丁丙诺啡液相色谱/质谱(LC/MS)分析方法。方法在含有丁丙诺啡的血浆中,加入内标奋乃静,加pH10.8缓冲溶液,用401有机担体作吸附剂、三氯甲烷作洗脱剂固相萃取,N2挥干,用50μL流动相定容后进行LC/MS分析。色谱条件:Thermo Hypersil-HyPURITY C18(150×2.1mm,5μm),柱温:40℃,流动相:10mmol/LNH4AC(pH3.4)∶甲醇∶乙腈=36∶52∶12,流速:0.22mL/min。结果方法的线性范围为0.05~5.0μg/L(r=0.9998),定量限0.05μg/L,检出限0.01μg/L(S/N=3);3个浓度的质量控制样品(0.1μg/L,0.5μg/L,2.0μg/L)平均回收率分别为86.40%,92.72%,92.57%,RSD分别为4.51%,3.34%,2.09%。结论该方法操作简便、灵敏度高,可用于涉毒案件血浆中丁丙诺啡的分析。

关 键 词:法医毒物分析  丁丙诺啡  固相萃取  液相色谱/质谱分析  血浆

A method for determination of buprenorphine in human plasma by high-performance liquid chromatography-mass spectrometry
LIU Dongxian,GONG Zhiping,CHEN Benmei. A method for determination of buprenorphine in human plasma by high-performance liquid chromatography-mass spectrometry[J]. Chinese Journal of Forensic Medicine, 2010, 25(3): 172-174
Authors:LIU Dongxian  GONG Zhiping  CHEN Benmei
Affiliation:(LIU Dongxian1,GONG Zhiping2,CHEN Benmei3/1. Department of Criminal Technology,Hunan Public Security College,Changsha 410138,China,2.Science & Technology Research Center,Department of Public Security of Hunan Province,Changsha 410001,3.Analysis Testing Center,Central South University,Changsha 410078,China)
Abstract:Objective To establish a sensitive and rapid method for determination of buprenorphine in human plasma by liquid chromatographic-electrospray ionization mass spectrometry. Methods Buprenorphine and perphenazine (IS) in plasma were absorbed with organic support 401 in buffer at pH10.8 and eluted with chloroform. After the chloroform was evaporated,the residue was dissolved in 50μL of mobile phase. The samples were separated using a Thermo Hypersil HyPURITY C18 reversed-phase column (150×2.1mm I.D.,5μm). A mobile phase containing of 10mmol/L ammonium acetate (pH=3.4)-acetonitrile-methanol (36:52:12,v/v/v) was used and isocratically eluted at a flow rate of 0.22mL/min.Buprenorphine and its internal standard,perphenazine,were measured by electrospray ion source in positive selective ion monitoring mode. Results The method was proved with good linearity ranged from 0.05~5.0μg/L with r=0.9998. The limit of quantification for buprenorphine in plasma is 0.05μg/L. The minimal limit of detection was 0.01μg/L(signal-noise:3:1). The mean extraction recoveries for the method were over 86.40%,92.72%,and 92.57% at concentration of 0.1,0.5,and 2.0μg/L,respectively. The precisions for the method were 4.51%,3.34%,and 2.09%,respectively. Conclusion This method is simple and sensitive determination of buprenorphine in human plasma in forensic practice.
Keywords:forensic toxicological analysis  buprenorphine  solid phase extraction  liquid chromatographic-mass pectrometric(LC/MS)  plasma  
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