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[目的]建立嘧菌酯合成工艺中的杂质分析方法,推测可能发生的副反应及其机理,为工艺优化和产品质量分析提供基础数据。[方法]选用嘧菌酯合成反应的混合物作为分析对象,以液质联用(LC/MS)定性采集各色谱峰的正负离子模式质谱信号。[结果]结合工艺背景信息,对所采集的质谱信号解析,得到了7种杂质结构,并根据结构特点推测了可能的副反应机理。[结论]该方法能够简单、快速测定嘧菌酯中的有机杂质,推测可能的副反应,灵敏度较高,适用于嘧菌酯生产过程监测及产品的质量控制。
[Objective] The research aimed to establish the impurity analysis method in azoxystrobin synthesis process, speculate the possible side reactions and its mechanism, and provide the basic data for process optimization and product quality analysis. [Method] The mixture of azoxystrobin synthesis reaction was selected as the analysis object, and the positive and negative ion mode mass spectrometry signals of each chromatographic peak were qualitatively collected by liquid chromatography-mass spectrometry (LC / MS). [Result] Seven kinds of impurity structures were obtained by analyzing the collected MS signals based on the background information of the process. The possible side reaction mechanism was deduced according to the structural characteristics. [Conclusion] This method could be used for the simple and rapid determination of organic impurities in azoxystrobin, speculated that the possible side reactions, high sensitivity, for the monitoring of azoxystrobin production process and product quality control.