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LC-MS法鑒定艾滋病治療藥物去羥肌苷的有關(guān)物質(zhì)

發(fā)布時(shí)間:2018-10-29 11:54
【摘要】:目的:采用高效液相色譜-質(zhì)譜聯(lián)用技術(shù)鑒定艾滋病治療藥物去羥肌苷的有關(guān)物質(zhì)結(jié)構(gòu)。方法:Inert Surstain C_(18)(250 mm×4.6 mm,5μm)色譜柱,以0.386%醋酸銨溶液加氨水調(diào)節(jié)p H至8.0為流動(dòng)相A,以甲醇-乙腈(50∶50)為流動(dòng)相B,進(jìn)行梯度洗脫,電噴霧正離子化高分辨TOF/MS和MS/MS檢測并解析有關(guān)物質(zhì)結(jié)構(gòu)。TOF/MS霧化氣壓力345 k Pa,溫度350℃,干燥氣流量10 L·min~(-1),毛細(xì)管電壓4 k V,碎片電壓100 V,MS/MS測定氬氣CID壓力0.2 Pa,碰撞能量25 e V。結(jié)果:檢測到去羥肌苷原料中共有8個(gè)有關(guān)物質(zhì),通過有機(jī)反應(yīng)機(jī)制分析和質(zhì)譜解析鑒定了他們的結(jié)構(gòu),他們分別是9-(2-氧基-丁酸)-1,4,5,7,8,9-六氫-嘌呤-6-酮、次黃嘌呤、肌苷、2′-去氧肌苷、9-(2-羥基-乙;)-1,9-雙氫-嘌呤-6-酮、3′-去氧肌苷、2′,3′-脫水肌苷、9-(2-羥乙基-4-丙酸甲酯-四氫呋喃)-1,9-雙氫-6H-嘌呤-6-酮。結(jié)論:采用色譜-質(zhì)譜聯(lián)用技術(shù)能有效地鑒定去羥肌苷的有關(guān)物質(zhì),可為其質(zhì)量控制研究提供參考。
[Abstract]:Objective: to identify the related substance structure of the AIDS treatment drug deshydroxyinosine by high performance liquid chromatography-mass spectrometry. Methods: Inert Surstain C _ (18) (250 mm 脳 4.6 mm,5 渭 m) column was used for gradient elution with 0.386% ammonium acetate solution and ammonia water as mobile phase A and methanol-acetonitrile (50:50) as mobile phase. The high resolution TOF/MS and MS/MS of electrospray ionization were used to detect and analyze the related material structures. The pressure of TOF/MS atomized gas was 345 k Pa, at 350 鈩,

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