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目的:对合成维生素E重要中间体三甲基氢醌工艺中所含的2个主要未知杂质进行结构解析。方法:采用等度洗脱高效液相色谱分析方法确定三甲基氢醌的杂质谱;通过两次半制备色谱方法及梯度洗脱分离出未知杂质1和杂质3;非挥发性目标物洗脱液浓缩采用减压旋转蒸发方法,挥发性目标物洗脱物采用固相萃取分离技术。杂质的精确分子量由高分辨质谱测定;杂质化学结构式采用高分辨一维和二维核磁共振谱进行结构解析。结果:两未知杂质经结构鉴定为2,5-二甲基氢醌和2,3,5-三甲基-2-环已烯-1,4-二酮,后者为首次报道。结论:本研究为易挥发性化学药物的有关物质结构解析提供了思路。
OBJECTIVE: To analyze the structure of two major unknown impurities contained in trimethylhydroquinone, an important intermediate of vitamin E synthesis. METHODS: The impurity profile of trimethylhydroquinone was determined by isocratic elution HPLC method. The unknown impurity 1 and impurity 3 were separated by two semi-preparative methods and gradient elution. The elution of non-volatile target Liquid concentration using a vacuum rotary evaporation method, the volatile target eluate solid phase extraction separation technology. The exact molecular weight of the impurity is determined by high-resolution mass spectrometry; the chemical structure of the impurity is resolved using high resolution 1D and 2D NMR spectroscopy. RESULTS: Two unknown impurities were identified as 2,5-dimethylhydroquinone and 2,3,5-trimethyl-2-cyclohexene-1,4-dione, the latter being the first reported. Conclusion: This study provides a way of thinking about the material structure of volatile chemicals.