高效液相色谱串联质谱法测定人血浆中硫辛酸

发布时间：2018-04-04 07:27

本文选题：维生素B类药物　切入点：硫辛酸　出处：《药物分析杂志》2015年01期

【摘要】：目的:建立LC-MS/MS法测定人血浆中硫辛酸浓度,并对口服0.2 g硫辛酸分散片后的药代动力学进行研究。方法:血浆样品以萘普生为内标,经乙腈沉淀蛋白后进行LC-MS/MS分析。采用高效液相分离系统,色谱柱为Venuseil XPB C18柱(150 mm×2.1 mm,5μm),流动相为乙腈-10 mmol·L-1醋酸铵-甲酸(80∶20∶0.2);采用质谱检测系统,ESI离子源,负离子模式,多反应监测(MRM)方式监测m/z 205→m/z 171(硫辛酸)和m/z 229→m/z 170(萘普生,内标)。结果:建立的LCMS/MS法在2.500~5 000 ng·m L-1质量浓度范围内,硫辛酸色谱响应与质量浓度相关性良好,定量下限为2.500 ng·m L-1;批内及批间精密度RSD均小于7%,准确度在96.5%~101.6%。12名受试者单次服用0.2 g硫辛酸分散片后AUC0-t为(1 816±885.6)ng·m L-1·h,AUC0-∞为(1 837±879.6)ng·m L-1·h,Cmax为(3 432±2 410)ng·m L-1,tmax为(0.45±0.44)h,t1/2为(0.45±0.18)h,MRT为(0.73±0.31)h,CL为(133.2±66.63)L·h-1,Vd为(85.60±50.98)L。结论:本测定方法灵敏准确,适用于人血浆中硫辛酸浓度的测定及其药代动力学研究。
[Abstract]:Objective: to determine the concentration of lipoic acid in human plasma by LC-MS/MS and Study on 0.2 g oral lipoic acid dispersible tablets after pharmacokinetics. Methods: plasma samples with Nai Pusheng as the internal standard, with acetonitrile protein precipitation was analyzed by LC-MS/MS. The phase separation system with high performance liquid chromatography column Venuseil XPB column (C18 150 mm * 2.1 mm, 5 m), acetonitrile -10 mmol L-1 ammonium acetate - formic acid (80: 20: 0.2); the mass detection system, ESI ion source, negative ion mode and multiple reaction monitoring (MRM) mode of monitoring m/z 205 to m/z 171 (lipoic acid) and m/z 229 m/z (Nai Pusheng, 170, internal standard). Results: the established LCMS/MS method in 2.500~5 000 ng m L-1 concentration range, lipoic acid concentration and chromatographic response relationship between the lower limit of quantification was 2.500 ng - M L-1; the intra batch and inter batch precision of RSD are less than 7% accuracy in 96.5%~101.6%.12 single subjects Taking 0.2 g lipoic acid dispersible tablet in AUC0-t (1816 + 885.6) ng - M L-1 - H, AUC0- - (1837 + 879.6) for ng - M L-1 - H, Cmax (3432 + 2410) ng, m L-1, Tmax (0.45 + 0.44) h, t1/2 (0.45 + 0.18) h, MRT (0.73 + 0.31) h, CL (133.2 + 66.63) L, H-1, Vd (85.60 + 50.98) L. conclusion: this method is sensitive and accurate, and suitable for the determination of drug concentration of lipoic acid in human plasma and pharmacokinetic studies.

【作者单位】：山东大学第二医院临床药学部;济南市疾病预防控制中心;山东大学药学院;
【基金】：山东大学第二医院青年基金项目资助(Y2013010075)
【分类号】：R96

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