中国临床药学杂志

目的考察4种前处理方法对采用液相色谱-串联质谱法(LC-Ms/Ms)定量分析人血浆中卤米松时基质效应的影响,以此来选择最佳前处理方法。方法人空白血浆加入低、中、高(1、10、20μg·L^-13种不同质量浓度水平的卤米松作为模拟血浆样品,地塞米松为内标,分别采用蛋白沉淀、液一液萃取、固相萃取和微固相萃取4种前处理方法,对测定结果的基质效应和提取回收率进行评价。结果采用微固相萃取OasisμElution装置进行样品前处理后,低、中、高3种模拟血浆样品的提取回收率分别为(91.61±O.20)%、(100.43±2.86)%和(102.80±5.83)%,方法经条件优化后的基质效应分别为(94.43±0.20)%、(86.55±2.86)%和(106.10±5.83)%。结论4种前处理方法中,微固相萃取法基质效应和提取回收率最佳,且操作简便、快速、灵敏度高、稳定性好,可用作卤米松的I临床血药浓度测定和药动学研究的样品前处理方法。

AIM To investigate the influence of four pretreatment methods on the matrix effect for determination of halometasone in human plasma by liquid chromatography-tandem mass spectrometry(LC-MS/MS).METHODS Before and after the pretreatment of human plasma via the methods of protein precipitation(PPT),liquid-liquid extraction(LIE),solid-phase extraction(SPE) and micro-solid-phase extraction(Oasis μElution),a certain concentration solution of halometasone was added exactly,and LC-MS/MS was adopted for sample analysis.Then,the matrix effects and the recoveries of halometasone in human plasma were evaluated.RESULTS The result showed that the mean recoveries and standard deviation of helametasone at low,medium and high concentrations were(91.61+0.20)%,(100.43 ~ 2.86)%and(102.80±5.83)%respectively and the matrix effects of blank plasma samples spiked after sample preprocessing with 1,10 and 20 μg·L^-1 of halometasone were found to be(94.43±0.20)%,(86.55±2.86)%and(106.10±5.83)%respectively by using Oasis μElution.CONCLUSION The Oasis μElution is the best pretreatment method of four both on the matrix effect and recoveries for determination of halometasone in human plasma by LC-MS/ MS.