高效液相色谱法分析精对苯二甲酸中的微量杂质

Determination of Micro Amount of Impurities in Purified Terephthalic Acid by High Performance Liquid Chromatography (HPLC)

应用高效液相色谱法，采用阴离子交换键合固定相，以磷酸盐缓冲溶液为流动相，ＵＶ２５４ｎｍ检测，外标法定量，同时测定了精对苯二甲酸（ＰＴＡ）中的主要杂质４－羧基苯甲醛（４－ＣＢＡ）和对甲基苯甲酸（ｐ－ＴＯＬ）的含量，４－ＣＢＡ和ｐ－ＴＯＬ的回收率分别为９８．３％～１０５．０％和９６．０％～１０３．８％，变异系数分别小于１．７％和３．３％。方法快速、准确，用于实际样品分析可得到满意的结果。

An HPLC method has been developed for simultaneous determination of micro amount of 4-caboxybenzaldehyde (4-CBA) and p-toluic acid (p-TOL)in purified terephthalic acid (PTA).These compounds were separated on a Spherisorb SAX column, 10μm, 250mm× 4.6mm i.d., or Shim-pack WAX-1 column, 3μm, 150mm×4. 0mm i- d., by using an acetonitrile-phosphate buffer solution(10:90, PH 4.3) as mobile phase, with UV detection at 254mn. The results have shown that the recoveries for 4-CBA and pTOL were 98. 3%￣ 105. 0% and 96. 0%￣ 103. 8% respectively and RSD were M 1.7% and <3.3%. The method has been applied to the determination of 4-CBA and P-TDL in PFA samples with satisfactory results.