LC-MS/MS分析人全血中五氟利多

Determination of penfluridol in human blood by LC-MS/MS

目的建立人体全血中五氟利多浓度的液相色谱-质谱联用法(LC-MS/MS)分析方法。方法全血中五氟利多和利培酮(内标)经正己烷液-液提取后,采用Capcell Pak C18色谱柱(250mm×2.0mm5,μm)进行分离,流动相为乙腈:20mmol/L乙酸胺和0.1%甲酸溶液(75∶25,V/V),流速为0.2mL/min,然后以MS/MS电喷雾正电离的多反应监测扫描方式(MRM)测定。用于定量分析的离子为m/z 524→109(五氟利多)和m/z 411→191(内标)。结果五氟利多的最低检测限为0.2ng/mL,在0.4～400ng/mL浓度范围内线性良好(r=0.9994),低、中、高浓度(1ng/mL、10ng/mL、100ng/mL)准确度分别为97%,108%和95%,日内和日间RSD均小于15%。结论该方法简便、快速、灵敏,适用于全血中五氟利多浓度的测定。

Objective To establish a LC-MS/MS method for determination of penfluridol in human blood.Methods Penfluridol and risperidone（internal standard） were isolated from human blood samples by liquid-liquid extraction with n-hexane,then chromatographed on a Capcell Pak C18 column（250mm×2.0mm,5μm） using a mobile phase consisted of acetonitrile/20mmol/L ammonium acetate containing 0.1% formic acid（75∶ 25,V/V）,at a flow rate of 0.2mL/min.A 4000 Q TRAP tandem mass spectrometer equipped with electrospray ionization source was used as detector and was operated in the positive ion mode.Multiple reaction monitoring（MRM） using the transitions m/z 524→109 and m/z 411→191 were used to quantify penfluridol and risperidone（IS）,respectively.Results The lower limit of detection of penfluridol was 0.2ng/mL,and the linear concentration range of the calibration curve for penfluridol was 0.4~400 ng/mL（r=0.9994）.The accuracies of low,medium and high concentrations（1ng/mL,10ng/mL,100ng/mL） were 97%,108% and 95%,respectively.The precision（RSD） of intra-day and inter-day was less than 15%.Conclusion The method was rapid,sensitive and suitable for qualitative and quantitative analysis of penfluridol in human blood.