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目的建立LC-MS/MS测定人血浆中盐酸哌甲酯的浓度。方法待测血浆1.0 mL,经1 mol.L-1的氢氧化钠40μL碱化后,用4 mL乙醚萃取处理,采用Eclipse XDB-C18(4.6 mm×150 mm,5μm)色谱柱,以甲醇和水为流动相梯度洗脱,流速1.0 mL.min-1。以电喷雾正离子源离子化,检测离子对盐酸哌甲酯为234.0/84.0,内标卡马西平为237.0/194.0。结果血浆中内源性物质对测定无干扰,最低定量限为0.1 ng.mL-1,在1~100 ng.mL-1内盐酸哌甲酯线性关系良好(r=0.999 1),日内、日间RSD均小于8%,样品分析时间为10 min。结论该法专属性强、灵敏度高,操作简便快速,测定结果可靠,适于进行盐酸哌甲酯血药浓度监测。
Objective To establish a LC-MS / MS method for the determination of methylphenidate in human plasma. Methods 1.0 mL plasma was prepared and then basified with 1 mol·L-1 sodium hydroxide (40 μL) and extracted with 4 mL diethyl ether. The column was eluted with Eclipse XDB-C18 (4.6 mm × 150 mm, 5 μm) Water as the mobile phase gradient elution, flow rate 1.0 mL.min-1. Ionization was performed on the electrospray positive ion source. The detected ion pair methylphenidate was 234.0 / 84.0, and the internal standard carbamazepine was 237.0 / 194.0. Results The plasma endogenous substance had no interference with the assay. The lowest limit of quantification was 0.1 ng.mL-1. The linear relationship was found between methylphenidate hydrochloride and 1 ~ 100 ng.mL-1 (r = 0.999 1) Inter-RSD was less than 8%, sample analysis time was 10 min. Conclusion The method is characterized by strong specificity, high sensitivity, simple and quick operation, reliable determination results and is suitable for the monitoring of methylphenidate blood concentration.