建立了一种利用高效液相色谱测定3,4,5-三甲氧基苯甲酸工业品中没食子酸含量的分析方法.在C18色谱柱(4.6×150 mm,5μm)上通过考察流动相种类、梯度起止比例及洗脱时间对保留的影响来优化色谱条件.最终以甲醇和0.1%高氯酸水溶液(v/v)为流动相,梯度洗脱程序:0 ~3 min,20%甲醇;3~8 min,20% ~ 65%甲醇;8~ 16 min,65%甲醇;紫外检测波长:270nm.实验结果表明,在优化的色谱条件下没食子酸在1.7 ×10-4 ~0.1 mg·mL-1范围内线性关系良好(r2=0.9999),日内和日间测定相对标准偏差分别为1.1%和1.3%,回收率在102.3% ~ 105.7%之间.此快速准确方法可用于3,4,5-三甲氧基苯甲酸工业品的质量控制.
A high performance liquid chromatographic (HPLC)method was established for determining the content of gallic acid in industrial 3,4,5 - trimethoxybenzoic acid product. The kinds of mobile phase and the gradient elution procedure were investigated on an ODS C18 column(4. 6 × 150 mm,5 μm)to optimize the chromatographic condition. Finally, we chose methanol ( A ) and 0. 1% perehloric acid aqueous solution ( B ) as mobile phases with gradient elution procedure :0 - 3 min ,20% A ;3 - 8 min ,20% A - 65% A ;8 - 16 min ,65% A. The detection wavelength was set at 270 nm. The gallic acid showed good linearity with correlation coefficient(r2) of 0. 9999 over the concentration from 1.7 μ10-4 mg · mL-1 to 0. 10 mg · mL-l. The intra-day and inter-day precisions were satisfactory with the relative standard deviations of 1.1% and 1.3 %, respectively. In addition, the recoveries of gallic acid were 102.3% - 105.7% at three spiked levels of 0. 2, 0. 3 and 0. 4 μg · mL- 1. this fast and precise HPLC method could be used in quality control in 3,4,5 - trimethoxy- benzoic acid for industrial use.