LC/MS分析血浆中丁丙诺啡

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。

A method for determination of buprenorphine in human plasma by high-performance liquid chromatography-mass spectrometry

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.