【摘要】 目的:建立LC-MS/MS法测定人唾液中维生素E醋酸酯的浓度。方法:在唾液中加入内标氘9-维生素E醋酸酯,用甲醇直接沉淀蛋白质法处理样品,Venusil XBP C8柱进行色谱分离;流动相为甲醇,流速0.8ml/min,柱温45℃,进样体积10μl;正离子多反应监测模式,离子通道分别为m/z473.4→207.4(维生素E醋酸酯)和482.4→216.4(氘9-维生素E醋酸酯)。结果:维生素E醋酸酯线性范围为5~5000μg/L,提取回收率为81.9%~93.9%,批内、批间精密度RSD均<10%,内标校正基质因子为0.99~1.0。结论:本方法操作简便,专一性好,灵敏度高,适用于维生素E醋酸酯补充剂临床用量监测,为药动学和药效学研究提供了参考。更多还原

【Abstract】 Objective:To establish a LC-MS/MS method for the concentration determination of vitamin E acetate in human saliva.Methods:After spiking isotope-labeled internal standards(d9-vitamin E acetate)into saliva,a direct protein precipitation was processed with methanol.Vitamin E acetate was separated on Venusil XBP C8 column with a mobile phase of methanol.The flow rate was 0.8ml/min and column temperature was kept at 45℃.The injection volume was 10μl.The protonated ions of analytes were detected in positive ionization through multiple reaction monitoring mode.The mass transition pairs of m/z473.4→207.4and 482.4→216.4were used to detect vitamin E acetate and d9-vitamin E acetate,respectively.Results:Vitamin E acetate displayed good linearity within the ranges of 5-5000μg/L.The extraction recovery rates were 81.9%-93.9%.The intra-batch and inter-batch relative standard deviation(RSD)was<10%.And the internal standard(IS)-matrix effect factors were within the ranges of 0.99-1.0.Conclusion:The established LC-MS/MS method is simple,specific and sensitive,and could be used to monitor the supplement of vitamin E acetate clinically and provide reference for pharmacokinetic and pharmacodynamic researches of vitamin E acetate.更多还原