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期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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LC-MS法鉴定艾滋病治疗药物去羟肌苷的有关物质

LC-MS identification of the degradation products of didanosine

作者(英文):
分类号:R917
出版年·卷·期(页码):2017,37 (11):1986-1993
DOI: 10.16155/j.0254-1793.2017.01.01
-----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:InertSurstain C18(250 mm×4.6 mm,5 μm)色谱柱,以0.386%醋酸铵溶液加氨水调节pH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 kPa,温度350℃,干燥气流量10 L·min-1,毛细管电压4 kV,碎片电压100 V,MS/MS测定氩气CID压力0.2 Pa,碰撞能量25 eV。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。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: To identify the related substances of didanosine by hyphenated LC-MS methods.Methods: The separation was carried out on InertSurstain C18(250 mm×4.6 mm, 5 μm) column with mobile phase consisting of 0.386% ammonium acetate solution(adjust pH=8.0 by amonia water solution) and methanol-acetonitrile(50:50) by gradient elution.The related substances were detected by positive ESI high resolution TOF/MS and their MS/MS spectra were determined as well.The conditions of TOF/MS were as follows:nebulizer pressure 345 kPa, gas temperature 350℃, drying gas flow 10 L·min-1, capillary voltage 4 kV and fragmentor100 V.The argon collision gas pressure of MS/MS was set at 0.2 Pa, and the collision energy at 25 eV.Results: There were 8 related substances in didanosine and their chemical structures were determined through the elucidation of their accurate TOF/MS data, the corresponding product MS spectra and further validated with the organic reaction mechanisms.The impurities were identified as 9-(2-oxo-4-butiric acid)-1, 4, 5, 7, 8, 9-hexahydro-purin-6-amine, hypoxanthine, inosine, 2'-deoxyinosine, 9-(2-hydroxy-acetyl)-1, 9-dihydrogen-purin-6-amine, 3'-deoxyinosine, 2', 3'-anhydroinosine, 9-(2-ethoxy-4-methyl propionate-tetrahydrofuran)-1, 9-dihydrogen-6H-purin-6-amine.Conclusion: The LC-MS method is useful for the identification of related substances in pharmaceuticals.The related substances found in didanosine are valuable for its quality control.

-----参考文献:---------------------------------------------------------------------------------------

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