【摘要】 目的建立人血浆中盐酸洛哌丁胺的液相色谱-质谱联用测定法(LC-MS/MS)。方法血浆样品中盐酸洛哌丁胺与盐酸小檗碱(内标)经甲醇液-液提取后,采用ZORBAX SB-C18色谱柱(2.1mm×150mm×5μm),柱温35℃,流动相为乙腈∶0.1%甲酸(60∶40,V/V),流速为0.4mL/min,进样量10μL。电喷雾离子源(ESI),正离子检测,以多反应监测(MRM)方式进行定量分析,用于监测的离子为m/z477→266(盐酸洛哌丁胺)和m/z366→292(内标)。结果盐酸洛哌丁胺的检测下限为0.2ng/mL(S/N=3),在浓度0.5~500ng/mL范围内线性良好(r=0.9982),低、中、高浓度(1ng/mL、20ng/mL、400ng/mL)的平均回收率分别为84.6%,88.5%和90.2%,日内与日间RSD分别小于6%与7%。结论LC-MS/MS法可用于盐酸洛哌丁胺的定性定量分析。更多还原

【Abstract】 Objective A LC-MS/MS method for analysis of loperamide hydrochloride in human plasma was developed.Methods Loperamide hydrochloride and berberine hydrochloride(internal standard) were separated from human plasma samples by liquid-liquid extraction with methanol.Chromatographic separation was performed on a ZORBAX SB-C18(2.1mm×150mm×5μm) column at 35℃.Acetonitrile/0.1% formic acid(60∶40 by volume) was used as mobile phase at a flow rate of 0.4mL/min,and the injection volume was 10μL.Electrospray ionization(ESI) source was applied and operated in positive ion mode.Quantification was performed using multiple reaction monitoring(MRM) of the transitions m/z 477→266 and m/z 366→292 for loperamide hydrochloride and the internal standard,respectively.Results The limit of detection of loperamide hydrochloride was 0.2ng/mL(S/N=3),and the calibration curve in the concentration range of 0.5～500ng/mL showed a good linear(r=0.9982).The average recoveries of low,medium and high concentrations(1ng/mL,20ng/mL,400ng/mL) were 84.6%,88.5% and 90.2%,respectively.The precisions(RSD) of winth-day and between-day were less than 6% and 7%,respectively.Conclusion This LC-MS/MS method can be used for qualitative and quantitative analysis of loperamide hydrochloride.更多还原