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目的建立测定人血浆中阿立哌唑浓度的反相高效液相串联质谱电喷雾检测法(LC-ESI-MS/MS)。方法以迪马C18反相柱(4.6mm×150mm,5μm)为色谱柱,流动相为甲醇-5mmol·L-1甲酸铵(90∶10),流速为1mL·min-1,柱温:25℃,以醋酸乙酯-二氯甲烷(4∶1)为提取剂。样品经电喷雾离子源正离子化后,通过三重四级杆串联质谱仪,采用选择反应监测(SRM)对阿立哌唑(m/z448.3→285.0)和内标替米沙坦(m/z515.3→497.3)进行测定。并用此法测定30例患者稳态血药浓度。结果阿立哌唑的高(400μg·L-1)、中(125μg·L-1)、低(10μg·L-1)3个质量浓度的平均回收率分别为94.27%、102.58%和97.97%,日内(n=5)、日间(n=3)RSD均小于15%;分析方法的最低定量限为1μg·L-1。线性范围为:5～500μg·L-1,回归方程为F=0.5469ρ+0.0714,r=0.999(n=7)。结论该方法灵敏、准确、简单、快速,可用于临床血浓监测和药动学研究。
Objective To establish a reversed-phase high performance liquid chromatography-tandem mass spectrometry (LC-ESI-MS / MS) method for the determination of aripiprazole in human plasma. Methods The mobile phase was methanol-5mmol·L-1 ammonium formate (90:10) at a flow rate of 1mL · min-1 using a Dima C18 reversed-phase column (4.6mm × 150mm, 5μm) ℃, with ethyl acetate - dichloromethane (4: 1) as extractant. Samples were electrospray ionized positive ionized by triple quadrupole mass spectrometer, selective reaction monitoring (SRM) of aripiprazole (m / z448.3 → 285.0) and the internal standard telmisartan (m /z515.3→497.3). The steady-state plasma concentration of 30 patients was determined by this method. Results The average recoveries of aripiprazole at the concentrations of 400μg · L-1, 125μg · L-1 and 10μg · L-1 were 94.27%, 102.58% and 97.97%, respectively. , Day (n = 5), daytime (n = 3) RSD were less than 15%, and the lowest limit of quantitation was 1μg · L-1. The linear range was 5 ~ 500μg · L-1, the regression equation was F = 0.5469ρ + 0.0714, r = 0.999 (n = 7). Conclusion The method is sensitive, accurate, simple and rapid and can be used in clinical blood concentration monitoring and pharmacokinetic studies.