摘要
目的建立LC-MS/MS法测定人血浆中利培酮及其代谢物9-羟基利培酮浓度的方法。方法血浆经特丁基甲醚提取,采用同位素内标(氘4-利培酮、氘4-9-羟基利培酮)进行测定。色谱柱:CAPCELL PACK C_(18)Ⅲ(100 mm×2.0 mm,5μm),流动相为乙腈-5 mmol·L^(-1)醋酸铵氨水缓冲液(pH=8)(50∶50,V/V),等度洗脱;流速0.4 mL·min^(-1);进样体积10μL;电喷雾离子化,正离子MRM扫描。结果利培酮及9-羟基利培酮线性范围均为0.1～50μg·L^(-1)(r>0.999 9),定量下限均为0.1μg·L^(-1),平均提取回收率均>80%,批内、批间精密度RSD均<10%。结论本方法灵敏度高、专一性好、操作简单,适用于利培酮的药动学研究。
AIM To develop a LC-MS/MS method for the determination of risperidone and the enantiomer of 9- hydroxyrisperidone in human plasma. METHODS The plasma samples were extracted with tert-butyl methyl ether and isotope-labeled internal standards （risperidone-d4 and 9-hydroxyrisperidone-d4） were used. The analytical column was CAPCELL PACK C18 m （100 mm × 2.0 mm, 5 tan）. The mobile phase, acetonitrile-ammonium buffer （ammonia water- 5 mmol·L^-1 ammonium acetate, pH 8） （50：50, V/V）, was used at a flow rate of 0.4 mL·min^-1. The injection volume was 10 μL. The protonated ions of analytes were detected in positive ionization by multiple reactions monitoring （MRM） mode. RESULTS The assay was validated from 0.1 to 50 μg·L^-1 （ r 〉 0.999 9） in plasma for all analytes. The lower limit of quantitation for all analytes was 0.1μg·L^-1 . The extraction recovery for all analytes was more than 80%. The intra-batch and inter-batch precision （RSD） were all less than 10%. CONCLUSION The established LC-MS/MS method is shown to be sensitive, accurate, simple and suitable for the pharmacokinetic research of risperidone.
出处
《中国临床药学杂志》
CAS
2010年第5期279-282,共4页
Chinese Journal of Clinical Pharmacy
基金
上海市科委科研计划项目(编号08411966700)资助
