高效液相色谱法测定色酚AS-PH反应液中三种组分的含量  

Detection of the contents of three major components in the reaction solution of naphthol AS-PH by High-performance liquid chromatography

作　　者：邢伶 王瑞菲 唐晓婵[1,2] 王艳[2] 岳涛[1,2] 冯维春 XING Ling;WANG Rui-fei;TANG Xiao-chan;WANG Yan;YUE Tao;FENG Wei-chun(Qingdao University of Science&Technology,Shandong Chemical Industry Research Institute,Jinan 250014,China;Chemical Technology Academy of Shandong Province,Organic Reaction in Aqueous Engineering Research Center of Shandong Province,Jinan 250014,China)

机构地区：[1]青岛科技大学山东化工研究院,山东济南250014 [2]山东省化工研究院山东省水相有机合成及高效清洁分离工程技术研究中心,山东济南250014

出　　处：《化学研究与应用》2020年第12期2281-2286,共6页Chemical Research and Application

基　　金：山东省政府“泰山学者”建设工程资金项目(08190201)资助。

摘　　要：建立了高效液相色谱法同时测定色酚AS-PH反应液中色酚AS-PH、邻氨基苯乙醚和2-羟基-3-萘甲酸含量的方法。色谱柱为Inert Sustain C18(4.6mm×150mm,5μm);检测波长为270nm;流动相为1g·L^-1磷酸二氢钾溶液(pH=3.0)-乙腈,梯度洗脱;流速为0.8mL·min^-1,外标法测定三种组分含量。结果表明:色酚AS-PH、邻氨基苯乙醚、2-羟基-3-萘甲酸与相邻色谱峰之间分离度良好,三种组分的浓度分别在2.0mg·L^-1~498mg·L^-1、2.0mg·L^-1~494mg·L^-1、1.0mg·L^-1~249mg·L^-1范围内线性关系良好,加标回收率分别为97.3%~103.7%、96.6%~102.0%、101.2%~104.6%。该方法操作简便、准确度高,可以为色酚AS-PH的工艺优化和中控分析提供依据。A high-performance liquid chromatography(HPLC)method was established for the determination of naphthol AS-PH,ophenetidine and 2-hydroxy-3-naphthoic acid in naphthol AS-PH reaction solution.Chromatographic experiments were performed on Inert Sustain C18 column(4.6 mm×150 mm,5μm),the mobile phase was 1g·L^-1 potassium dihydrogen phosphate solution(pH=3.0)and acetonitrile in gradient elution,the flow rate was 0.8 mL·min^-1 and the detection wavelength was 270 nm,the contents were calculated by external reference method.The results showed that naphthol AS-PH,o-phenetidine and 2-hydroxy-3-naphthoic acid peaks were completely separated from adjacent peaks,and the three components had good linear relationships between 2.0mg·L^-1~498mg·L^-1、2.0mg·L^-1~494mg·L^-1、1.0mg·L^-1~249mg·L^-1 respectively,three levels standard were added to reaction solutions and the recoveries were 97.3%~103.7%、96.6%~102.0%、101.2%~104.6%respectively.The proposed method was simple and suitable for accurate determination of naphthol AS-PH,o-phenetidine and 2-hydroxy-3 naphthoic acid in naphthol AS-PH reaction solution,which would provide precise data for processing optimization and middle control analysis.

关 键 词：高效液相色谱法 色酚AS-PH 邻氨基苯乙醚 2-羟基-3-萘甲酸 反应液 

分 类 号：O657.7[理学—分析化学]