高效液相色谱-串联质谱法测定人血浆中雷沙吉兰的浓度  

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

作　　者：施柳茜 张全英[1,2] 周文佳[2] 

机构地区：[1]苏州大学医学部药学院,江苏苏州215123 [2]苏州大学附属第二医院Ⅰ期临床试验研究室,江苏苏州215004

出　　处：《中国临床药理学杂志》2016年第10期924-926,共3页The Chinese Journal of Clinical Pharmacology

摘　　要：目的建立高效液相色谱质谱联用(HPLC-MS/MS)法测定人血浆中雷沙吉兰的浓度。方法以司来吉兰作为内标,色谱柱用XterraRP18(4.6mm×100 mm,3.5μm),流动相由乙腈与20 mmo L·L^(-1)醋酸铵水溶液(含0.01%甲酸)组成,梯度洗脱,流速为1000μL·min^(-1),多反应监测(MRM)模式,电喷雾离子源(ESI),正离子检测。生物样品预处理用乙腈直接沉淀蛋白。结果雷沙吉兰血浆浓度在0.01~15.00 ng·m L^(-1)线性关系良好,批内精密度相对标准偏差(RSD)<10.90%,批间精密度RSD<10.10%,提取回收率在98.07%~100.39%,基质效应在93.18%~94.64%。结论该法准确、灵敏度高、重现性好,可用于健康受试者口服甲磺酸雷沙吉兰片和外贴雷沙吉兰透皮贴片的人体药代动力学研究。Objective To establish a high performance liquid chromatography-tandem mass spectrometry method（ HPLC-MS /MS） for the quantification of rasagiline in human plasma.Methods Selegiline was used as internal standard.The separation was performed on the Xterra RP18colunm（ 4.6 mm × 100 mm,3.5 μm） with the mobile phase consisted of acetonitrile and 20 mmo L·L^-1ammonium acetate containing0.01% formic acid at a flow rate of 1000 μL·min-（-1）under gradient elution within 6.5 min.Electrospray ionization（ ESI） source was applied and operated in multiple reaction monitoring（ MRM） mode via positive ionization.Plasma samples were pretreated by acetonitrile precipitation.Results A good linearity of rasagiline was obtained in the concentration range of 0.01-15.00 ng·m L^-1.The inter and intra-batch precision was less than 10.90% and 10.10%,respectively.The percentage recoveries ranged from 98.07% to 100.39% and matrix effect ranged from 93.18% to 94.64%.Conclusion The method is sensitive,accurate,reproducible and suitable for the study of pharmacokinetics of rasagiline in healthy Chinese volunteers after a single dose of rasagiline mesylate tablet and patches.

关 键 词：雷沙吉兰 高效液相色谱质谱联用法 药代动力学 

分 类 号：R971.5[医药卫生—药品]