| 替加氟有关物质的色谱-质谱结构鉴定 |
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| 引用本文： | 王敏,金婵,卢萍,丁娅,杭太俊. 替加氟有关物质的色谱-质谱结构鉴定[J]. 中国现代应用药学, 2015, 32(1): 62-66 |
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| 作者姓名： | 王敏 金婵 卢萍 丁娅 杭太俊 |
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| 作者单位： | 中国药科大学,中国药科大学,中国药科大学,中国药科大学,中国药科大学 |
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| 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。
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| 关 键 词： | 替加氟 有关物质 色谱-质谱联用 |
| 收稿时间： | 2014-03-14 |
| 修稿时间： | 2014-07-02 |
Identification of the Related Substances in Tegafur with Hyphenated Techniques |
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| WANG Min,JIN Chan,LU Ping,DING Ya and HANG Taijun. Identification of the Related Substances in Tegafur with Hyphenated Techniques[J]. The Chinese Journal of Modern Applied Pharmacy, 2015, 32(1): 62-66 |
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| Authors: | WANG Min JIN Chan LU Ping DING Ya HANG Taijun |
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| Affiliation: | China Pharmaceutical University,China Pharmaceutical University,China Pharmaceutical University,China Pharmaceutical University,China Pharmaceutical University |
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| Abstract: | ABSTRACT: OBJECTIVE The study aims to identify the related substances in tegafur by hyphenated techniques. The hyphenated LC-MS method is used for the identification of related substances in tegafur and the results obtained are valuable 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 10mM 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 |
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| Keywords: | tegafur related substances LC-TOF/MS LC-MS/MS |
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