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目的:采用高效液相色谱-串联质谱(HPLC-MS/MS)和高效液相色谱-二极管阵列检测(HPLC-PDA)法对双苯氟嗪中的杂质进行结构分析。方法:采用C18柱,甲酸铵溶液(用甲酸调节pH至3.2)-甲醇为流动相,线性梯度洗脱,流速0.5 mL.min-1,柱温45℃,MS/MS和PDA分别检测。结果:双苯氟嗪中的主要杂质有效分离,通过解析获取的质谱和紫外信息,结合原料合成工艺,对其中3个未知杂质的结构进行了推断。结论:本实验分离鉴别了双苯氟嗪中的主要杂质,为双苯氟嗪的质量控制和工艺优化提供了参考。
OBJECTIVE: To analyze the impurities in dipfluzine by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) and high performance liquid chromatography-diode array detection (HPLC-PDA) Methods: C18 column, ammonium formate solution (adjusted to pH 3.2 with formic acid) -methanol was used as the mobile phase. The mobile phase was eluted with a linear gradient of 0.5 mL.min-1. The column temperature was 45 ℃. Results: The main impurities in dipfluzine were effectively separated. The structures of three unknown impurities were inferred by analyzing the obtained mass spectra and UV information, combined with the synthesis of raw materials. Conclusion: The main impurities of dipfluzine were separated and identified in this experiment, which provided reference for the quality control and process optimization of dipfluzine.