HPLC间接测定电氧化合成中的茴香醛二甲基缩醛

Indirect Determination of Anisaldehyde Dimethyl Acetal in the Process of Electrochemical Oxidation Synthesis by HPLC

在无水KF-CH3OH体系中直接电氧化合成的茴香醛二甲基缩醛(p-MBDMA)遇水易发生水解。研究表明在甲醇、乙腈和水的酸性混合溶液中,p-MBDMA在色谱柱中能迅速彻底地水解为茴香醛,故利用其水解反应建立了一种间接测定p-MBDMA的高效液相色谱(HPLC)方法。选择最佳流动相为水-甲醇-乙腈(50:30:20),用磷酸调节pH值至3.0,并探讨了测定机理。建立的HPLC测定方法准确、可靠,已应用于电化学合成p-MBDMA的分析,并可满足工业化生产的分析要求。

The anisaldehyde dimethyl acetal（p-MBDMA） that produced by direct electrochemical oxidation synthesis in the anhydrous KF-CH3OH system is easily hydrolyzed in water.The study results indicated that p-MBDMA could be hydrolyzed into anisaldehyde raidly and completely in the acidic mixed solution of methanol,acetonitrile and water.Based on this,a high performance liquid chromatographic（HPLC） method was developed for the determination of p-MBDMA indirectly.The best mobile phase was a mixture of water-methanol-acetonitrile（50：30：20,adjusted pH 3.0 by phosphoric acid）.The internal mechanism of p-MBDMA in the column was also investigated.The results showed that HPLC method could be successfully applied in the rapid determination of p-MBDMA content.