高效液相色譜串聯(lián)質(zhì)譜法同時檢測人血漿伊馬替尼及代謝物
發(fā)布時間:2018-05-15 07:42
本文選題:伊馬替尼 + N-去甲伊馬替尼; 參考:《中國醫(yī)院藥學(xué)雜志》2017年21期
【摘要】:目的:建立一種同時測定人血漿中伊馬替尼及其活性代謝產(chǎn)物N-去甲基伊馬替尼的高效液相色譜串聯(lián)質(zhì)譜(HPLCMS/MS)法,并應(yīng)用于檢測胃腸間質(zhì)瘤患者伊馬替尼及代謝物的濃度。方法:血漿樣品經(jīng)甲醇沉淀蛋白后,以含0.1%甲酸的水溶液和甲醇溶液為流動相;采用梯度洗脫,Waters ACQUITY UPLC BEH C18(2.1 mm×50 mm,1.7μm)色譜柱進行分離,流速為0.3 m L·min~(-1);柱溫為35℃。ESI離子源,正離子模式,多反應(yīng)監(jiān)測,用于定量分析的離子對為m/z 494.2→m/z 394.3(伊馬替尼)、m/z 480.3→m/z 394.3(N-去甲基伊馬替尼)、m/z 502.5→m/z 394.4(內(nèi)標,伊馬替尼-D8)。結(jié)果:伊馬替尼和N-去甲伊馬替尼的線性范圍均為50~10 000 ng·mL~(-1),定量下限為50 ng·mL~(-1),伊馬替尼及代謝物的準確度分別為97.9%~109.0%,95.5%~103.5%,日內(nèi)和日間變異系數(shù)10%。結(jié)論:本方法簡便、準確、靈敏、專屬性強,適用于人血漿中伊馬替尼及其代謝物濃度的檢測。
[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,
本文編號:1891590
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