液相色谱-串联质谱法测定人血浆中的利培酮

[Determination of risperidone in human plasma by liquid chromatography-tandem mass spectrometry].

作者信息

Duan Xiao-tao, Chen Xiao-yan, Zhang Yi-fan, Zhong Da-fang

机构信息

Center for Drug Metabolism Research, Shanghai Institute of Materia Medica, Chinese Academy of Sciences, Shanghai 201203, China.

出版信息

Yao Xue Xue Bao. 2006 Jul;41(7):684-8.

PMID:17007366

Abstract

AIM

To develop and validate a liquid chromatographic-tandem mass spectrometric (LC-MS/MS) method for the determination of risperidone in human plasma.

METHODS

Risperidone and the internal standard, diphenhydramine, were isolated from plasma by liquid-liquid extraction with etherdichloromethane (3:2, v/v) , then chromatographed on a Zorbax Extend-C18 column (150 mm x 4.6 mm ID, 5 microm) using a mobile phase consisted of acetonitrile-water-formic acid (40:60: 0.5, v/v), at a flow rate of 0.7 mL x min(-1). A Finnigan TSQ tandem mass spectrometer equipped with atmospheric pressure chemical ionization source was used as detector and was operated in the positive ion mode. Selected reaction monitoring (SRM) using the precursor product ion combinations of m/z 411-->191 and m/z 256-->167 were used to quantify risperidone and diphenhydramine (IS) , respectively.

RESULTS

The linear concentration range of the calibration curve for risperidone was 0.025 - 50 microg L(-1). The lower limit of quantification was 0.025 microg x L(-1). The intra- and inter-day relative standard deviation (RSD) across three validation running over the entire concentration range was less than 7.1%. The accuracy was within +/- 3.8%. Each sample was chromatographed within 2.7 min.

CONCLUSION

The method was proved to be rapid, sensitive and suitable for pharmacokinetic investigations of risperidone.

摘要

目的

建立并验证一种用于测定人血浆中利培酮的液相色谱-串联质谱（LC-MS/MS）方法。

方法

利培酮和内标苯海拉明通过用乙醚-二氯甲烷（3:2，v/v）液-液萃取从血浆中分离出来，然后在Zorbax Extend-C18柱（150 mm×4.6 mm内径，5μm）上进行色谱分析，流动相由乙腈-水-甲酸（40:60:0.5，v/v）组成，流速为0.7 mL·min⁻¹。配备大气压化学电离源的Finnigan TSQ串联质谱仪用作检测器，以正离子模式运行。分别使用m/z 411→191和m/z 256→167的前体产物离子组合进行选择反应监测（SRM）来定量利培酮和苯海拉明（内标）。