HPLC-MS/MS法测定人血浆中千金藤素的浓度  

Determination of cepharanthine in human plasma by HPLC-MS/MS

作　　者：郭智[1] 王丹[2] 刘冰洋[2] 刘颖[2] 刘婷立[2] 宋冬梅[2] 

机构地区：[1]内蒙古医学院附属医院药物临床试验机构,内蒙古010050 [2]沈阳亿灵医药科技有限公司,沈阳110179

出　　处：《实用药物与临床》2013年第6期514-517,共4页Practical Pharmacy and Clinical Remedies

基　　金：沈阳亿灵中药创新药物孵化基地(2011ZX09401-016)

摘　　要：目的建立人血浆中千金藤素浓度的HPLC-MS/MS测定法。方法血浆样品1.0 mL经甲基叔丁基醚萃取后,以2.5 mmol/L醋酸铵(含0.05%甲酸)-甲醇(40∶60)为流动相,采用ZORBAX Eclipse XDB-C8(150 mm×4.6 mm,5μm)柱分离,采用电喷雾电离化(ESI)方式和多反应离子监测(MRM)模式进行正离子检测。用于定量分析的离子反应分别为m/z 607.2→365.1(千金藤素)和m/z 247.2→98.0(内标甲哌卡因)。结果千金藤素血药浓度线性范围为0.10～208.40 ng/mL,定量下限为0.10 ng/mL。低、中、高3个浓度提取回收率分别为72.3%、76.8%、79.5%。结论该法操作简便、快速、灵敏,适用于千金藤素在人体内的药代动力学研究。Objective To develop a high-performance liquid chromatography coupled to tandem mass spectrometry（HPLC-M S / M S） method for the quantification of cepharanthine in human plasma.Methods Cepharanthine and the internal standard（I.S.）,mepivacaine w ere extracted from human plasma by methyl tert-butyl ether.Cepharanthine and mepivacaine separation w as performed on a ZORBAX Eclipse XDB-C8（150 mm × 4.6 mm,5 μm） column and detected by tandem mass spectrometry.The mobile phase consisted of 2.5 mmol / L ammonium acetate（include 0.05% formic acid w ater）-methanol（40∶ 60）.Detection and quantitation w as performed by M S / M S using electrospray ionization（ESI） and multiple reaction monitoring（M RM） in the poditive ion mode.The most intense[M ＋ H]＋（MRM） trasitions of cepharanthine at m/z 607.2→365.1 was used for quantitation and the transition at m/z 247.2 → 98.0 w as used to monitor mepivacaine.Results The linear calibration curve w as obtained in the concentration range of 0.10 ～ 208.40 ng / mL.The limit of quantification w as 0.10 ng / mL.The extraction recoveries of the three concentrations（low / moderate / high） were 72.3%,76.8%,79.5% respectively.Conclusion The method is proved to be suitable for the clinical investigation of cepharanthine pharmacokinetics with the advantages of specificity,speed and greater sensitivity.

关 键 词：千金藤素 血药浓度 HPLC-MS MS 

分 类 号：R96[医药卫生—药理学]