高效液相色谱-大气压化学电离源-质谱法测定人血浆中帕洛诺司琼浓度

Determination of palonosetron in plasma by HPLC-APCI-MS

目的:建立液质联用法(HPLC-MS/MS)测定人血浆中帕洛诺司琼浓度的方法。方法:色谱条件为Hypersil GOLD(150.0 mm×4.6 mm,5μm)柱,流动相为0.2%醋酸铵水溶液(含0.1%甲酸)-甲醇(50∶50),质谱条件为大气压化学电离源(AP-CI源),血浆样品中加入内标,碱化后用乙酸乙酯提取,浓缩后采用高效液相色谱-质谱联用进行测定。结果:血浆样品中帕洛诺司琼浓度在0.04～20.00 ng/ml的线性范围内关系良好(r=0.999 9),定量下限为0.04 ng/ml;低、中、高浓度的回收率、批内及批间精密度均符合生物样本测定方法学要求。结论:本方法灵敏度高、专属性强、重现性好,可用于帕洛诺司琼药代动力学研究及血药浓度监测。

Objective：To establish a determination method of palonosetron level in plasma.Methods：LC conditions were as follows：Hypersil GOLD（150 mm × 4.6 mm,5 μm）was used with the mobile phase consisting of acetateamine buffer（0.1% formic acid）-method（50∶50）.Equipped with an atmospheric pressure chemical ionization（APCI）source was used as detector.The plasma samples added with internal standard were extracted with Acetic Ether,then concentrated and determined by LC-MS /MS.Results：The linear range of palonosetron was 0.04～20.00 ng /ml.The lower limit of quantification（LLOQ）was 0.04 ng /ml.The recoveries of palonosetron at low,middle and high concentration and the intra-day and inter-day RSDs all met the standards.Conclusion：The established method is sensitive,specific,reproducible and suitable for studies of pharmacokinetics and detection of plasma drug concentration of palonosetron.