LC-MS/MS测定人血浆中哌甲酯

LC-MS/MS Determination of Methylphenidate in Human Plasma

关键词:  LC-MS/MS  盐酸哌甲酯  药动学

Key words:  LC-MS/MS  methylphenidate hydrochloride  pharmacokinetics

摘要:

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40 μL碱化后，用4 mL乙醚萃取处理，采用Eclipse XDB-C₁₈ (4.6 mm×150 mm，5 μm)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。

Abstract:

OBJECTIVE To establish an LC-MS/MS method for determination of methylphenidate in human plasma. METHODS 1.0 mL plasma was basified with 40 μL 2 mol·L^-1 NaOH and extracted with 4 mL ether. The separation was performed on an Eclipse XDB-C₁₈ column (150 mm×4.6 mm, 5 μm). The mobile phase consisted of methanol and water for gradient elution. Methylphenidate was determined by LC-MS/MS operated in the positive ion mode. RESULTS The limit of quantitation was 0.1 ng·mL^-1, and a good linearity was obtained in the range of 1–100 ng·mL^-1(r=0.999 1). The RSD of inter-day and intra-day precision were less than 8%. Each analysis was completed within 10 min. CONCLUSION The method is accuracy, sensitive and simple, proved to be suitable for the study of therapeutic drug monitoring of methylphenidate.