目的 研究盐酸雷洛昔芬的杂质谱,为质量标准制定提供依据。方法 采用高效液相色谱-离子阱-飞行时间质谱联用技术分析盐酸雷洛昔芬破坏后的样品及杂质对照品,研究各杂质的来源,并根据已知杂质的质谱裂解规律,对未知杂质的结构进行推定。结果 盐酸雷洛昔芬经破坏后,共产生3个杂质,其中1个为未知杂质。雷洛昔芬及其杂质的质谱裂解呈现很强的规律性,据此推测未知杂质为雷洛昔芬进一步氧化生成的砜。结论 本实验深入研究了盐酸雷洛昔芬的杂质谱,对盐酸雷洛生产过程中杂质的控制与体内药物分析具有指导意义。
Abstract
OBJECTIVE To investigate the impurity profile of raloxifene thus to lay a foundation for the establishment of drug quality standard. METHODS HPLC-IT-TOF-MS was adopted to analyze destroyed raloxifene and reference substances of impurities. According to the mass spectrometry fragmentation patterns of known impurities,the structures of unknown impurities were speculated. RESULTS Destroyed raloxifene totally produced three impurities,one of which was unknown. Based on the regular mass spectrometry fragmentation patterns of raloxifene and known impurities,the unknown impurity was speculated to be a sulfone that was generated through further oxidation of raloxifene. CONCLUSION The methods and results of this study could lay a foundation for the impurity control during production and in vivo analysis of raloxifene.
关键词
雷洛昔芬 /
杂质谱 /
裂解规律 /
质量控制 /
液质联用
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Key words
raloxifene /
impurity profile /
fragmentation pattern /
quality control /
HPLC-IT-TOF-MS
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中图分类号：
R917
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参考文献
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