高效液相色谱串联质谱法同时检测人血浆伊马替尼及代谢物
发布时间:2018-05-15 07:42
本文选题:伊马替尼 + N-去甲伊马替尼 ; 参考:《中国医院药学杂志》2017年21期
【摘要】:目的:建立一种同时测定人血浆中伊马替尼及其活性代谢产物N-去甲基伊马替尼的高效液相色谱串联质谱(HPLCMS/MS)法,并应用于检测胃肠间质瘤患者伊马替尼及代谢物的浓度。方法:血浆样品经甲醇沉淀蛋白后,以含0.1%甲酸的水溶液和甲醇溶液为流动相;采用梯度洗脱,Waters ACQUITY UPLC BEH C18(2.1 mm×50 mm,1.7μm)色谱柱进行分离,流速为0.3 m L·min~(-1);柱温为35℃。ESI离子源,正离子模式,多反应监测,用于定量分析的离子对为m/z 494.2→m/z 394.3(伊马替尼)、m/z 480.3→m/z 394.3(N-去甲基伊马替尼)、m/z 502.5→m/z 394.4(内标,伊马替尼-D8)。结果:伊马替尼和N-去甲伊马替尼的线性范围均为50~10 000 ng·mL~(-1),定量下限为50 ng·mL~(-1),伊马替尼及代谢物的准确度分别为97.9%~109.0%,95.5%~103.5%,日内和日间变异系数10%。结论:本方法简便、准确、灵敏、专属性强,适用于人血浆中伊马替尼及其代谢物浓度的检测。
[Abstract]:Aim: to establish a high performance liquid chromatography-tandem mass spectrometry (HPLCMS / MS) method for simultaneous determination of imatinib and its active metabolite in human plasma, and to determine the concentration of imatinib and its metabolites in patients with gastrointestinal stromal tumors (GIST). Methods: the plasma samples were precipitated by methanol and separated by gradient elution of Waters ACQUITY UPLC BEH C182.1 mm 脳 50 mm ~ (1.7 渭 m) column at a flow rate of 0.3 mL / min ~ (-1) with a column temperature of 35 鈩,
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