LC-MS/MS同时测定人血浆中的利培酮和9-羟基利培酮  

Determination of Risperidone and 9-hydroxyrisperidone in human plasma by LC-MS/MS

作　　者：李红霞[1] 杨东菁[2] 范頔[3] 王雪芹[4] 邢向伟[5] 

机构地区：[1]河南省肿瘤医院药剂科,河南郑州450003 [2]河南大学医学院,河南开封475001 [3]河南科技大学动物科技学院,河南洛阳471003 [4]河南省食品药品检验所,河南郑州450003 [5]河南中医学院,河南郑州450003

出　　处：《华西药学杂志》2011年第4期369-371,共3页West China Journal of Pharmaceutical Sciences

摘　　要：目的采用LC-MS/MS法检测人血浆中的利培酮及其活性代谢产物9-羟利培酮。方法采用BEH C18色谱柱(50mm×2.1 mm,1.7μm),流动相A相为乙腈、B相为0.01 mol.L-1醋酸铵(甲酸调pH3.4),梯度洗脱,流速0.2 mL.min-1,柱温45℃,进样量3μL。利培酮、9-羟利培酮及盐酸丁螺环酮内标的检测离子对分别为:m/z 411.42→191.19、427.45→207.18、386.43→122.27。结果利培酮、9-羟利培酮的线性范围分别为0.66～42.24、0.65～41.60 ng.mL-1(r=0.997,n=5);在人血浆基质中,高、中、低浓度(1.3、5.2、21.12 ng.mL-1)的日内、日间RSD均小于15%;利培酮、9-羟利培酮方法的回收率分别为89%～109%、97%～107%。6份不同来源的血浆基质效应研究证实,该样品预处理方法对血浆中的利培酮和9-羟利培酮测定无干扰。结论所建方法处理简单、灵敏、特异性高,定量准确,可为利培酮制剂的临床药物动力学研究提供分析方法。OBJECTIVE To establish a method for determination of Risperidone and 9-hydroxyrisperidone in human plasma by HPLC-MS/MS.METHODS BEH C18（50 mm×2.1 mm,1.7 μm）,the mobile phase consisted of A（acetonitrile） and B（0.01 mol·L-1 ammonium acetate）（formic acid adjust pH3.4）,gradient elution at flow rate of 0.2 mL·min-1,column temperature was 45 ℃,and inject volume 3 μL.With positive ion MRM detection of Risperidone（m/z 411.42→191.19）,and 9-hydroxyrisperidone（m/z 427.45→207.18）,using Buspirone hydrochloride（m/z 386.43→122.27） as internal standard,respectively.RESULTS A good linearity was obtained in the range of risperidone 0.66-42.24 ng·mL-1（r=0.997,n=5）and 9-hydroxyl-Risperidone 0.65-41.60 ng·mL-1（r=0.997,n=5）with 9-hydroxyrisperidone＇s intra-day RSD and inter-day RSD were less than 15%.The recovery was within 89%-109% and 97%-107%.Plasma matrix effect test showed endogenous matrix had no effect on quantification of Risperidone and 9-hydroxyrisperidone.CONCLUSION A rapid,sensitive and accurate LC-MS/MS method was developed for the determination of Risperidone and 9-hydroxyrisperidone in human plasma.

关 键 词：利培酮 9-羟利培酮 高效液相串联质谱法 血药浓度 

分 类 号：R969[医药卫生—药理学]