替加氟有关物质的色谱-质谱结构鉴定

Identification of the Related Substances in Tegafur with Hyphenated Techniques

关键词:  替加氟  有关物质  色谱-质谱联用

Key words:  tegafur  related substances  LC-MS/MS

摘要:

目的 采用色谱-质谱联用技术鉴定替加氟有关物质，为其工艺和质量控制提供参考依据。方法 采用十八烷基硅烷键合硅胶的填充剂，流动相为乙腈-甲醇-10 mmol·L^-1醋酸铵缓冲溶液，对替加氟有关物质进行分离；采用电喷雾正离子化-飞行时间质谱法测定各有关物质的准确质量，三重四极杆质谱测定子离子特征，并经解析鉴定各杂质结构。结果与结论 替加氟与其有关物质分离良好，检测出4个主要有关物质均为替加氟合成的起始原料，是母核基本未发生变化，仅5位被不同基团取代的衍生物。

Abstract:

OBJECTIVE To identify the related substances in tegafur by hyphenated techniques for its manufacturing process and quality control. METHODS A column packed with the octadecyl silane chemically bonded silica was used for the separation of the related substances with a mixture of acetonitrile-methanol and 10 mmol·L^-1 ammonium acetate buffer solution as the mobile phase by isocratic elution. The structures of the related substances were speculated and identified by electrospray positive ionization LC-TOF/MS accurate ion mass and MS/MS determination and elucidation. RESULTS & CONCLUSION Tegafur and the related substances are separated under the established HPLC condition. Four related substances in tegafur are characterized by hyphenated techniques. Their structures are elucidated as the different substituents having the same frame structure as tegafur and starting material.