LC/MS/MS分析人血浆中利培酮和9-OH-利培酮的浓度

Determination of the Concentration of RIS in Human Plasma and 9-OH-RIS With LC/MS/MS

目的：建立高效液相-质谱联用法测定人血浆中利培酮和9-OH-利培酮的浓度。方法：液相：色谱柱为Hypurity C18柱（Thermo Hypersil-Keystone 2．1mm×150mm，5μm）；流动相为乙腈：1‰甲酸=85：15；流速为0．2ml·min^-1；柱温为40℃，自动进样瓶温10℃。质谱：离子源为ESI源，源电压5．0KV；加热毛细管温度275℃；鞘气（N2）流速30ml·min^-1；辅助气流速5ml·min^-1；正离子方式检测；扫描方式为选择反应监测（SRM），用于定量分析的离子分别为219（内标左羟丙哌嗪）、191（利培酮）和207（9-羟基-利培酮）。结果：利培酮（RIS）线性范围为0．1～50ng·ml^-1，最小检出浓度为0．05ng·ml^-1。9-羟基-利培酮线性范围为0．1～50ng·ml^-1，最低检出浓度为0．05ng·ml^-1。提取回收率均大于50％。日内、日间RSD均小于10％。结论：本方法简便、灵敏、准确，可用于利培翻和9-0H-利培酮血药浓度检测和药代动力学研究。

Objective： To the HPLC - mass spectra method for determination of the concentration of risperidone（RIS） in human plasma and 9- OH- RIS. Method： （1）liquid phase： the chromato bar was Hypurity C18 column; mobile phase was acetonitrile ： 1‰formic acid = 8 ： 15; flow rate： 0.2ml · min^-1 ; column temperature： 40℃ ; bottle temperature： 10℃. （2） Mass spectra： ion source： ESI source, source voltage： 5.0KV, heating capillary temperature：275℃ ; N2 ： ml · min^-1, assist air current speed： 5ml · min^-1 ; poison style was used to detect; the scanner mode was SRM, the ions of quantitative analysis were 219, 191,207 respectively. Result： the linear range of RIS was 0.1 -50ng · ml^-1 ; the lowest detection concentration was 0.05ng · ml^-1 ; the two targets of 9 - OH - RIS was same the RIS. The abstractive recovery was higher than 50%. The RSD of Inner a day and among days was lower than 10%. Conclusion： the method was simple, sensitive, accurate, can be used to determine the concentration of RIS and 9 - OH - RIS in blood and study pharmacokinetics.