4-(2-萘)苯硼酸频那醇酯的高效液相色谱分析方法

Analysis of 4-(2-Naphthalene) phenylborate Pinacol Ester by HPLC

因硼原子存在空的P轨道,硼酸频那醇酯类化合物容易受到带孤对电子的亲核试剂的进攻而水解,难以保证化合物始终维持原有的分子状态。同时硼酸酯类化合物对热不稳定,用气相色谱(GC)测定难以得到准确结果。本文以4-(2-萘)苯硼酸频那醇酯为分析对象,用以下液相色谱条件进行分析:流动相为乙腈,色谱柱为Venusil XBP C184.6mm×50mm×5μm(3根串联),溶剂为四氢呋喃,柱温为40℃,流速为1.0mL·min^(-1),检测波长为260nm,进样量为5μL,总分析时间30min。分析结果显示,主峰保留时间为12.8min,主峰峰形良好,杂质分离度高,方法重现性良好。

Boric acid pinacol ester compounds were easy to be hydrolyzed by nucleophiles with lone pair electrons due to the existence of empty P orbitals of boron atoms,which was difficult to ensure that the compounds always maintained their original molecular state.In addition,borate esters were thermally unstable,and it was difficult to obtain accurate results by gas chromatography(GC).In this paper,pinacol 4-(2-naphthalene)phenylborate ester was analyzed under the following liquid chromatographic conditions:acetonitrile was mobile phase,chromatographic column was venusil XBP C184.6mm*250mm*5μm(three columns in series),solvent was tetrahydrofuran,column temperature was 40℃,flow rate was 1.0mL/min,detection wavelength was 260nm,injection volume was 5μL,the total analysis time was 30min.The results showed that the retention time of the main peak was 12.8min,and the shape of the main peak was good,the separation of impurities was high,and the reproducibility of the method was good.