杂多酸盐催化苯酚羟基化制备苯二酚反应产物的反相高效液相色谱分析

Reversed-phase HPLC determination of related dihydric phenols in phenol hydroxylation catalyzed by heteropolyacid salts

建立了反相高效液相色谱法测定杂多酸盐催化苯酚羟基化制备苯二酚反应产物的分析方法.样品经稀释和经滤膜过滤处理后,在Shim-pack CLC ODS色谱柱(4.6 mm i.d.×150 mm,5μm)上,以甲醇-水(V(甲醇):V(水)=35:65)+体积分数1%乙酸为流动相,流速为1.0 mL/min,柱温为40℃,紫外检测波长280nm,8 min内可以将对苯二酚、邻苯二酚和苯酚完全分离并定量,三者的线性范围分别为0.01～0.60,0.01～0.50,0.05～1.00mg/mL.反应后在及时分析样品的前提下,该法适合进行苯酚羟基化的产物分析.

A reversed phase high performance liquid chromatographic method for the determination of reaction products in the phenol hydroxylation using heteropoly acid salt catalysts was established. After samples were diluted and filtrated through membrane, hydroquinone, catechol and phenol can be completely separated and determined with UV detector at 280 nm within 8 min on a Shim-pack CLC ODS column（4.6 mm i.d. × 150 mm,5 μm） at 40℃ . The mobile phase composition was methyl/water （35/65）added by 1% acetic acid with a flow rate of 1.0 mL/min. The linear ranges of hydroquinone, catechol and phenol were found to be 0.01 - 0.60 mg/mL,0.01 - 0.50 mg/mL,0.05- 1.00 mg/mL, respectively. This method was proved to be a convenient and fast way with high precision suitable for the product analysis of phenol hydroxylation.