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液相色谱-质谱联用法快速测定人血浆中加巴喷丁浓度

Rapid determination of gabapentin concentration in human plasma by liquid chromatography-mass spectrometry
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摘要 目的采用LC-MS/MS法测定人血浆中加巴喷丁的药物浓度。方法血浆样品经甲醇沉淀蛋白后,以乙腈∶5mmoL/L醋酸铵水溶液(含0.3%甲酸)=10∶90(v/v)为流动相,经Waters Symmetry C18(3.9×150mm,5μm)色谱柱分离,样品经大气压力化学离子源正离子化后,通过三重四极杆串联质谱仪,在多反应监测模式下测定加巴喷丁(m/z 172.1→154.1)和内标左乙拉西坦(m/z 171.1→126.1)的浓度。结果加巴喷丁的血浆浓度在20.00~8000.00ng/mL范围内线性良好,定量下限为20.00ng/mL,批内、批间精密度(RSD)均在2.3%~10.9%以内,相对偏差(RE)在±15%范围内。加巴喷丁低浓度质控血浆样品提取回收率结果为(102.3±4.4)%,中浓度质控血浆样品提取回收率结果为(97.5±2.6)%,高浓度质控血浆样品提取回收率结果为(99.7±2.0)%,内标左乙拉西坦提取回收率结果为(98.7±3.0)%。结论该分析方法简便、特异性高、灵敏度高,可用于人血浆中加巴喷丁的浓度检测。 Objective To determine the concentration of gabapentin in human plasma through the LC-MS/MS method.Methods After protein was precipitated from plasma samples through methanol,the plasma samples were separated on Waters Symmetry C18(3.9×150mm,5μm)column with acetonitrile∶5mmoL/L ammonium acetate aqueous solution(containing 0.3%formic acid)=10∶90(v/v)as mobile phase.After the samples were positively ionized through atmospheric pressure chemical ion source,the concentrations of gabapentin(m/z 172.1→154.1)and internal standard(IS)levetiracetam(m/z 171.1→126.1)were determined by triple quadrupole tandem mass spectrometer in a multi-reaction monitoring mode.Results The linearity of gabapentin plasma concentration was good in the range of 20.00 to 8000.00ng/mL,the lower limit of quantification was 20.00ng/mL,the RSD(relative standard deviation)of within-run precision and between-run precision was both between 2.3%and 10.9%,and the relative error(RE)was within the range of±15%.The extraction recovery rate of gabapentin low-concentration quality control plasma sample was(102.3±4.4)%,that of gabapentin medium-concentration quality control plasma sample was(97.5±2.6)%,that of gabapentin high-concentration quality control plasma sample was(99.7±2.0)%,and that of IS levetiracetam was(98.7±3.0)%.Conclusion The analysis method is simple,specific and sensitive.It can be used for the determination of the concentration of gabapentin in human plasma.
作者 徐凤华 孙晓鸣 XU Fenghua;SUN Xiaoming(Department of Pharmacy,the Affiliated Suzhou Science&Technology Town Hospital of Nanjing Medical University,Jiangsu,Suzhou 215153,China)
出处 《中国医药科学》 2020年第15期41-44,64,共5页 China Medicine And Pharmacy
基金 江苏省苏州市药学会—江苏恒瑞临床药学科研基金项目(Syhky201807) 江苏省苏州市科技发展计划项目(SYSD2018228)。
关键词 加巴喷丁 血药浓度 高效液相-串联质谱方法 测定 Gabapentin Plasma concentration High-performance liquid chromatography-tandem mass spectrometry Determination
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