摘要
目的建立一种简便、灵敏的测定人体血浆和尿液中帕洛诺司琼浓度的高效液相色谱一串联质谱（HPLC-MS／MS）方法。方法血浆、尿液样品分别采用甲醇沉淀处理后，选样分析。采用Agilent-ZORBAX-C18色谱柱（2．1mm×50mm，5fμm）．以乙腈-0．1％甲酸溶液为流动相，采用正离子，多反应监测方式测定样品浓度。用于定量分析的检测离子质荷电（m／z）297．2→m/z110．1（帕洛诺司琼）和DI／Z285．0→M／z193．0（内标）。结果帕洛诺司琼血浆样品在0．02～10ng·mL^-1与峰面积线性关系良好（r=0．9975）；定量下限（LLOQ）为0．02ng·L^-1；日内与日间RSD均〈10％；回收率在89．6％～114．0％。尿样在2．5～100ng·mL^-1与峰面积线性关系良好，7—0．9974；定量下限（LLOQ）为2．5ng·mL^-1；日内与日间RSD均〈10％；回收率在96．4％～113．4％。结论本方法简便快速、灵敏准确，适用于帕洛诺司琼在人体体内的药物动力学研究。
Objective To establish a simple, sensitive high performance liquid chromatography tandem mass spectrometry （HPLC-MS/MS） method to determine palonosetron in human plasma and urine. Methods The plasma and urine samples were precipitated by methanol and then were injected directly into the HPLC MS/MS system. Agilent-ZORB AX C18 （2. 1 mm × 50 mm, 5 μm） column was used with acetonitrile-0.1% formic acid water solution as mobile phase by gradient elution. Palonosetron and the internal standard, diazepam, were separated by HPLC and quantitated by MS/MS using electrospray ionization and multiple reaction monitoring in the positive ion mode. The most intense [M-H]- MRM transition of palonosetron at m/z 297.2→m/z 110.1 was used for the quantitation and the transition at m/z 285. 0→m/z 193.0 was used to monitor diazepam. Results The minimal detectable plasma concentration was 0.02 ng· mL ^-1, and the calibration curve was linear at 0. 02 10 ng · mL^-1 （r=0. 997 5）. The average recovery was between 89.6% and 114.0%. Intra-day and inter-day RSD was less than 10%. The minimal detectable urine concentration was 2.5 ng · mL ^-1, the calibration curve was linear at 2.5 100 ng ·mL ^-1 （r=0. 997 4）. The average recovery was between 96.4% and 113.4% Intra-day and inter-day RSD was less than 10%. Conclusion The method is simple, sensitive and accurate. It is suitable for the study of pharmacokinetics of palonosetron in human plasma and urine.
出处
《中南药学》
CAS
2010年第2期119-123,共5页
Central South Pharmacy
