LC-MS法鉴定艾滋病治疗药物去羟肌苷的有关物质

发布时间：2018-10-29 11:54

【摘要】：目的:采用高效液相色谱-质谱联用技术鉴定艾滋病治疗药物去羟肌苷的有关物质结构。方法:Inert Surstain C_(18)(250 mm×4.6 mm,5μm)色谱柱,以0.386%醋酸铵溶液加氨水调节p H至8.0为流动相A,以甲醇-乙腈(50∶50)为流动相B,进行梯度洗脱,电喷雾正离子化高分辨TOF/MS和MS/MS检测并解析有关物质结构。TOF/MS雾化气压力345 k Pa,温度350℃,干燥气流量10 L·min~(-1),毛细管电压4 k V,碎片电压100 V,MS/MS测定氩气CID压力0.2 Pa,碰撞能量25 e V。结果:检测到去羟肌苷原料中共有8个有关物质,通过有机反应机制分析和质谱解析鉴定了他们的结构,他们分别是9-(2-氧基-丁酸)-1,4,5,7,8,9-六氢-嘌呤-6-酮、次黄嘌呤、肌苷、2′-去氧肌苷、9-(2-羟基-乙酰基)-1,9-双氢-嘌呤-6-酮、3′-去氧肌苷、2′,3′-脱水肌苷、9-(2-羟乙基-4-丙酸甲酯-四氢呋喃)-1,9-双氢-6H-嘌呤-6-酮。结论:采用色谱-质谱联用技术能有效地鉴定去羟肌苷的有关物质,可为其质量控制研究提供参考。
[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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