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.
作者
邢伶
王瑞菲
唐晓婵
王艳
岳涛
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)
出处
《化学研究与应用》
CAS
CSCD
北大核心
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。
