高效液相色谱测定单偶氮染料合成中的原料及中间体

Analysis of Main Components in the Synthesis of Monoazo-dyes by High Perofrmance Liquid Chromatography

采用高效液相色谱法,对以甲酸铬、4-氯-2-氨基苯酚和2-萘酚为原料合成反应产物单偶氮染料进行分析,以体积比为80∶16∶3∶1的乙腈-水-乙酸-三乙胺为流动相,C18柱为固定相,紫外检测器检测波长为313nm。实验探讨了色谱柱、流动相及pH值等因素对分离效果的影响,确定了最佳色谱条件。该法对甲酸铬、4-氯-2-氨基苯酚、2-萘酚、反应中间体及单偶氮染料的检出限(S/N=3)分别为0.30、0.12、0.17、0.21、0.05g·L-1,这五种组分回收率为95.9%～102.5%,相对标准偏差(RSD)为0.65%～4.16%。该方法简便快速,准确度高,可用于实际生产质量控制分析。

High perofrmance liquid chromatography was applied for the determination of monoazo-dyes produced from chromic formate,4-chloro-2-aminophenol and 2-naphthol.A solution composed of acetonitrile,water,acetic acid and triethylamine（80＋16＋3＋1,by volume）was used as mobile phase. C18column and UV-detector at 313nm were included in the chromatographic conditions.The influence of chromatographic column,mobile phase and pH value on the separation were investigated,and the optimum analtyical conditions were obtained.The limits of detection for chromic formate,4-chloro-2-aminophenol,2-naphthol,intermediate product and monoazo-dyes were 0.30,0.12,0.17,0.21and 0.05g/L^-1,respectively.The recovery was in the range of 95.9～102.5%,and the RSD was among 0.66‰～4.16‰.The method was simple,reproducible,and applied to the analysis of real samples with satisfactory results.