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本文建立了一种快速、高灵敏的HPLC-MS/MS法用于检测人血浆中的草乌甲素浓度。血浆样品采用沃特斯HLB小柱进行固相萃取,汉邦C18色谱柱(150 mm×4.6 mm,5μm)进行分离,流动相为甲醇∶水(85∶15,v/v),水相含10 mmol/L的醋酸铵和0.1%的甲酸。采用ESI源和多反应监测(MRM)的方式进行检测,草乌甲素及内标的反应离子对分别为644.4/584.4和237.2/194.2,草乌甲素血药浓度在0.010～1.0 ng/mL范围内线性关系良好,最低定量限为0.010 ng/mL可以满足口服0.4 mg草乌甲素后血药浓度的检测,日内日间及质控样品精密度及准确度均在允许范围内。本检测方法被成功的应用在中国健康志愿者生物等效性研究中,20名志愿者口服0.4 mg草乌甲素试验制剂和参比制剂后主要药代动力学参数分别如下:Cmax(0.325±0.110),(0.323±0.115)ng/mL;AUC0-16(1.627±0.489),(1.732±0.556)ng.h/mL;AUC0-∞(1.730±0.498),(1.831±0.562)ng.h/mL;t1/2(4.26±0.95),(3.80±0.90)h;Tmax(1.34±0.54),(1.83±0.99)h。
In this paper, a rapid and sensitive HPLC-MS / MS method was developed for the determination of the concentration of abacavirin in human plasma. The plasma samples were separated on HLB C18 column (150 mm × 4.6 mm, 5 μm) using Waters HLB cartridges. The mobile phase consisted of methanol: water (85:15, v / v) 10 mmol / L ammonium acetate and 0.1% formic acid. The ESI and multi-reaction monitoring (MRM) methods were used to detect the concentrations of abamectin and internal standard 644.4 / 584.4 and 237.2 / 194.2 respectively. The concentration of abamectin in the range of 0.010-1.0 ng / mL Within the linear relationship between the minimum limit of quantification of 0.010 ng / mL to meet the oral concentration of 0.4 mg of Aconite plasma concentration test, day and day quality control samples and accuracy are within the allowable range. The test method was successfully applied in the bioequivalence study of healthy volunteers in China. The main pharmacokinetic parameters of 20 volunteers after oral administration of 0.4 mg of arachidin test preparation and reference preparation were as follows: Cmax (0.325 ± AUC0-16 (1.627 ± 0.489), (1.732 ± 0.556) ng.h / mL; AUC0-∞ (1.730 ± 0.498), (1.831 ± 0.562) ng.h / mL; t1 / 2 (4.26 ± 0.95), (3.80 ± 0.90) h; Tmax (1.34 ± 0.54), (1.83 ± 0.99) h.