高效液相色谱法同时测定豆制品中4种对羟基苯甲酸酯的研究

Simultaneous analysis of four p-hydroxybenzoate preservatives in soybean products by high-performance liquid chromatography

目的:建立豆制品中对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯和对羟基苯甲酸丁酯等防腐剂的高效液相色谱同时测定方法。方法:样品经甲醇/水(50∶50,V/V)提取后,采用C18色谱柱,以乙酸-乙酸铵缓冲液(0.02 mol/L,pH=5.5)/乙腈为流动相,采用梯度洗脱分离,在紫外226 nm波长进行检测。结果:4种对羟基苯甲酸酯的加标回收率在87.0%~99.8%范围,其相对标准偏差在1.6%~4.9%范围,在0.1 mg/L^25.0 mg/L范围均具有良好的线性,其回归系数均大于0.999,检出限(LOD)均为0.2 mg/kg,最低定量检出限(LOQ)为0.7 mg/kg。结论:本方法简便、灵敏、重现性好,能满足豆制品中对羟基苯甲酸酯类残留的监测要求。

Objective：To set up an assay for the simultaneous analysis of four p-hydroxybenzoate preservatives,such as methylparaben,ethylparaben,propyl p-hydroxybenzoate and butyl p-hydroxybenzoate in soybean products by high-performance liquid chromatography.Methods： After the p-hydroxybenzoates were extracted by methanol/water（50∶50,V/V）,the sample was separated on a C18 column by a mobile phase consisting of ammonium acetate-acetate acid（0.02 mol/L,pH=5.5）/acetonitrile in gradient elution.Detection was carried out by an ultraviolet detector at 226 nm.Results： Calibration curves of the four preservatives were linear within the range of 0.1 mg/L^25.0 mg/L with correlation coefficients of more than 0.999,the limits of detection（LOD） were 0.2 mg/kg,and the limits of quantification（LOQ） were 0.7 mg/kg.The extraction recoveries were between 87.0%~99.8%,and the RSDs were between 1.6%~4.9%.Conclusion： This method is simple,sensitive,and accurate,and was suitable for monitoring the p-hydroxybenzoates residues in soybean products.