摘要
目的建立人血浆中奥洛他定浓度测定的液相色谱-串联质谱(LC-MS/MS)定量方法。方法以地氯雷他定为内标,血浆样品经蛋白沉淀处理后,在0.2 mL·min-1的流速下以乙腈-甲醇-0.1%甲酸水溶液(25:5:70,V/V/V)为流动相进行等度洗脱,采用CAPCELL PAK C_(18)柱(50 mm×2.1 mm,3.5μm)分离。样品经电喷雾离子源(ESI)正离子化后,通过三重四极杆串联质谱仪,采用多反应离子检测方式测定奥洛他定(m/z 338.2/165.2)和内标地氯雷他定(m/z 311.1/259.1)的浓度。结果奥洛他定质量浓度在1～200μg·L^(-1)内线性良好,定量下限为1μg·L^(-1),方法回收率为85%～115%,批内、批间RSD均<10%。结论本方法专属性强、灵敏度高,操作简便、快速,符合生物样品分析要求,适用于临床药动学研究。
AIM To develop a liquid chromatography-tandem mass spectrometry （LC-MS/MS） method for determination of olopatadine in human plasma after oral administration of olopatadine hydrochloride tablet. METHODS Plasma samples were treated by protein precipitation using desloratadine as internal standard. The separation of olopatadine and its internal standard was performed on a CAPCELL PAK C18 column with mobile phase（aeetonitrile-methanol-0.1% formate, 25 ： 5 ： 70, V/V/V） run at 0.2 mL· min^- 1. A triple quadrupole tandem mass spectrometer was used as detector. Electrospray ionization source was applied and operated in positive ion mode. In multiple reaction monitoring, the Q1/Q3 ion transitions of m/z 338.2/165.2 and m/z 311.1/259.1 were used to quantify olopatadine and desloratadine, respectively. RESULTS The calibrated linear curve was ranged from μg· L^- 1 to 200μg· L^- 1 with the detection limit of 1 μg·L^-1 in human plasma. The method recovery was within 85% - 115%, and the relative standard deviation of within-batch and between-batch was less than 10%. CONCLUSION The method proved to be specific, sensitive and rapid for evaluating the pharmacokinetics of olopatadine.
出处
《中国临床药学杂志》
CAS
2009年第6期338-341,共4页
Chinese Journal of Clinical Pharmacy
关键词
奥洛他定
液相色谱-串联质谱法
血浆药物浓度
olopatadine
liquid chromatography-tandem spectrometry
plasma drug concentration
