高效液相色谱-串联质谱法对家兔血浆中奥司他韦浓度的测定  

Determination of Oseltamivir in Rabbit Plasma by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：洪爱华[1] 李满妹[2] 刘忠[3] 梁志红[1] 

机构地区：[1]暨南大学分析测试中心,广东广州510632 [2]暨南大学中药及天然药物研究所,广东广州510632 [3]暨南大学生物医药基地,广东广州510632

出　　处：《分析测试学报》2010年第2期131-135,共5页Journal of Instrumental Analysis

基　　金：广东省自然科学基金资助项目(07005971);暨南大学引进优秀人才科研启动基金资助项目(51209005)

摘　　要：建立了家免血浆中奥司他韦的高效液相色谱-串联质谱测定方法。以ZORBAXXDB—C18柱为色谱柱，乙腈-0．4％甲酸水溶液为流动相，梯度洗脱；流速300μL·min-1；柱温：20℃。质谱条件为气动辅助电喷雾离子源（ESI），检测方式为正离子多离子反应监测（MRM），以m／z313／166、313／208为定性离子对，m／z313／166为定量离子；生物样品采用固相萃取方法处理。奥司他韦的线性范围为0．05—500μg·L-1，定量下限达0．05μg·L-1，日内、日间相对标准偏差均小于6％，回收率为91％～93％，结果表明该法准确、灵敏、特异，适用于生物样品中奥司他韦的测定。该文还进一步探讨了奥司他韦主要质谱碎片的产生机理。A bioanalytical method for analysis oseltamivir in rabbit plasma using a high performance liquid chromatography coupled to tandem mass spectrometry （ HPLC - MS/MS ） has been developed and validated. The separation of osehamivir was performed on a ZORBAX XDB-C18 column （50 mm × 2. 1 mm, 5 μm）with a mobile phase of acetonitrile -0.4% formic acid at flow rate of 300 μL . min- 1 The column temperature was set at 20℃. The detection of oseltamivir was carried out under the positive electrospray ionization and multiple reaction monitoring （MRM） mode. The transition of m/z 313/166 and m/z 313/208 was used for qualitative analysis, in which m/z 313/166 was selected as quantitative analysis. The plasma samples were extracted by solid phase extraction. The calibration curve of oseltamivir was linear in the range of 0. 05 - 500 μg . L-1 with a limit of quantitation of 0. 05 μg . L-1 The within-day and between-day RSDs were less than 6% and the recoveries was in the range of 91% -93%. The results showed that the method was accurate, sensitive and specific, and was suitable for determination of oseltamivir in biological sample. The colli- sion-active dissociation pathway of oseltamivir were also discussed by MS/MS/MS technique.

关 键 词：高效液相色谱-串联质谱 奥司他韦 血浆 碰撞活化裂解 

分 类 号：O657.72[理学—分析化学] R917[理学—化学]