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应用高效液相色谱方法研究了以2,6二氯苯酚和苯胺为起始原料合成药物中间体1(2,6二氯苯基)2吲哚酮(DCI)过程中,DCI及相关物质在不同色谱条件下的分离情况。结果表明,以CLCCN(150mm×6.0mmi.d.,7μm)为分离柱,以MeOHH2O(体积比为6∶4)为流动相,在流速为1mLmin的情况下,DCI及相关物质可以达到基线分离。建立了快速准确测定DCI纯度和检验杂质种类的高效液相色谱分析方法,方法准确可靠。对两个精品和两个粗品分别进行测定,结果表明精品中的杂质主要为N(2,6二氯二苯胺基)氯乙酰胺,粗品中的杂质主要为N(2,6二氯二苯胺基)氯乙酰胺和2,6二氯二苯胺。
The high performance liquid chromatography (HPLC) method was used to study the synthesis of drug intermediate 1 (2,6-dichlorophenyl) 2-indolone (DCI) using 2,6-dichlorophenol and aniline as raw materials. Separation under different chromatographic conditions. The results showed that with CLCCN (150mm × 6.0mmi.d., 7μm) as the separation column and MeOHH2O (6: 4) as the mobile phase, DCI and related substances could be separated at baseline at a flow rate of 1mLmin . A rapid and accurate HPLC method for the determination of DCI purity and impurities was established. The method was accurate and reliable. The results of two products and two crude products showed that the main impurities in the products were N (2,6-dichlorodianilino) chloroacetamide. The impurities in the crude product were mainly N (2,6-dichlorodiphenylamine Yl) chloroacetamide and 2,6 dichlorodiphenylamine.