LC-MS/MS法测定人血浆中丙戊酸钠的浓度

Determination of sodium valproate in human plasma by LC- MS /MS

目的建立LC-MS/MS法定人血浆中丙戊酸钠浓度的方法。方法以霉酚酸为内标,血浆样品经甲醇直接沉淀蛋白后,用迪马C18色谱柱(4.6 mm×150 mm,5μm)进行分离,以0.1%乙酸铵-乙腈(42∶58)为流动相,流速1.0mL·min-1,柱温30℃,用多离子监测(Q1)方式进行检测。结果丙戊酸钠的线性范围为1.0～150.0μg·mL-1;最低检测限为0.1μg·mL-1。高、中、低3个浓度的日内RSD小于3%,日间RSD小于10%,绝对回收率均大于75%。结论本法简便、快速、灵敏、重现性好,能够有效的检测人血浆丙戊酸钠的含量。

Objective To establish a LC - MS/MS method for the concentration of sodium valproate （VPA） in human plasma. Methods Myeophenolic acid was used as internal standard. After one step protein precipitation,the analysis was chromatographed on C18 （4.6 mm × 150 mm,5μm）. An isocratic mobile phase consisted of 0. 1% ammonium acetate in water- aeetonitrile （42：58）. Flow rate was 1.0 mL · min-1, column temperature was 30℃. Detection was carried out by multiple reaction monitoring （MRM） on a 3200 QTRAP LC - MS/MS system. Results The calibration curves of each drug showed a good linearity in a range of concentration between 1.0- 150.0 μg ·mL-1 for sodium valproate,r = 0. 997 3. Intra and inter precision （ RSD% ） were less than 3% and 10% , respectively. The recoveries were above 75%. Conclusion The method is simple, rapid, sensitive, which is suitable for determination of sodium valproate in human plasma.