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建立了二维液相色谱法测定明胶空心胶囊中对羟基苯甲酸甲酯(1)、对羟基苯甲酸乙酯(2)、对羟基苯甲酸丙酯(3)和对羟基苯甲酸丁酯(4)。对羟基苯甲酸酯先在线富集于Boton C_(18)色谱柱顶端,然后转移至TSK Gel ODS C_(18)色谱柱进行分离。以0.02 mol/L乙酸铵溶液和甲醇为流动相,梯度洗脱,检测波长254 nm。在上述条件下1~4分离完全,且在0.25~2.5mg/ml范围内线性关系良好。平均回收率分别为99.9%、99.4%、98.8%和99.2%,RSD分别为1.9%、2.0%、1.5%和2.2%。
A two-dimensional liquid chromatography was developed for the determination of methylparaben (1), ethylparaben (2), propylparaben (3) and butylparaben 4). Parabens were first concentrated online on the top of a Boton C_ (18) column and then transferred to a TSK Gel ODS C_ (18) column for separation. With 0.02 mol / L ammonium acetate solution and methanol as mobile phase, the gradient elution was carried out. The detection wavelength was 254 nm. 1 ~ 4 under the above conditions completely separated, and in the range of 0.25 ~ 2.5mg / ml good linear relationship. The average recoveries were 99.9%, 99.4%, 98.8% and 99.2%, respectively, with RSDs of 1.9%, 2.0%, 1.5% and 2.2%, respectively.