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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。
Objective To establish a liquid chromatography-tandem mass spectrometry (LC-MS / MS) quantitative method for the determination of the concentration of olopatadine in human plasma. Methods Plasma desmetazidine was used as an internal standard. The plasma samples were precipitated with protein and treated with acetonitrile-methanol-0.1% aqueous solution of formic acid (25: 5: 70, V / V / V ) Was used as the mobile phase for isocratic elution, using a CAPCELL PAK C_ (18) column (50 mm × 2.1 mm, 3.5 μm). The samples were ionized by electrospray ionization (ESI), and olotetine (m / z 338.2 / 165.2) and internal standard desloratadine were determined by multi-reactive ion detection using a triple quadrupole tandem mass spectrometer (m / z 311.1 / 259.1). Results The linearity of olopatadine was within 1 ~ 200 μg · L -1 with the lower limit of quantification being 1 μg · L -1. The recovery rate was 85% ~ 115%. Intra-assay and inter-assay RSD All <10%. Conclusion The method is highly specific, sensitive and easy to operate. It is in accordance with the requirements of biological sample analysis and is suitable for clinical pharmacokinetic studies.