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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
【摘要】 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Hypu-rity C18柱(Thermo Hypersil-Keystone 2.1mm×150mm,5μm);流动相为乙腈:1‰甲酸=85:15;流速为0.2m l.m in-1;柱温为40℃,自动进样瓶温10℃。质谱:离子源为ESI源,源电压5.0 KV;加热毛细管温度275℃;鞘气(N2)流速30m l.m in-1;辅助气流速5m l.m in-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(R IS)线性范围为0.1~50ng.m l-1,最小检出浓度为0.05ng.m l-1。9-羟基-利培酮线性范围为0.1~50ng.m l-1,最低检出浓度为0.05ng.m l-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,可用于利培酮和9-OH-利培酮血药浓度检测和药代动力学研究。
【Abstract】 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=815;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.
- 【文献出处】 中医药导报 ,Guiding Journal of TCM , 编辑部邮箱 ,2006年05期
- 【分类号】R96
- 【被引频次】2
- 【下载频次】190