高效液相色谱法测定精对苯二甲酸中微量杂质

Determination of Trace Impurity in Terephthalic Acid by High Performance Liquid Chromatography

中文关键词:  高效液相色谱  精对-苯二甲酸  4-羧基苯甲醛  对甲基苯甲酸  苯甲酸

英文关键词:high performance liquid chromatography  terephthalic acid  4-carboxybenzaldehyde  p-toluic acid  benzoic acid

中文摘要:

      建立了高效液相色谱法(HPLC)同时测定精对-苯二甲酸(PTA)中微量杂质4-羧基苯甲醛(4-CBA)、对甲基苯甲酸(P-TOL)和苯甲酸(C₇H₆O₂)含量的方法.采用的色谱柱为Shim-Pack WAX-1柱,流动相为0.1mol/LNH₃H₂PO₄+6%CH₃OH,(pH4.5),检测波长为254nm.PTA中微量杂质4-CBA、P-TOL和C₇H₆O₂的含量分别为0.59～235.20mg/kg、4.52～392.00mg/kg和0.28～24.55mg/kg时线性关系良好,其线性相关系数分别为0.9998、0.9997和0.9999.苯甲酸加样平均回收率99.03%,RSD0.37%.

英文摘要:

      The contents of trace impurity 4-Carboxybenzaldehyde(4-CBA)、p-Toluic acid(p-TOL) and Benzoic acid(C₇H₆O₂) intere phthalic acid by high performance liquid chromatography(HPLC) were determined. A Shim-Pack WAX-1 column was used with the mobile phase of 0.1 mol/L NH₃H₂PO₄+6%CH₃OH(pH 4.5) and the detection wavelength was 254 nm. The trace impurity calibration curves had good linearity in range of 0.59～235.20 mg/kg、4.52～392.00 mg/kg and 0.28～24.55 mg/kg and the correlation coefficients were 0.999 8、0.999 7 and 0.999 9 for 4-CBA、p-TOL and C₇H₆O₂ respectively, the average recovery b enzoic acid added was 99.03% (n=6) and RSD was 0.37%.