优化气相色谱法测定酱油中对羟基苯甲酸酯类含量的方法

Method for determining the content of parabens in soy sauce by optimized gas chromatography

目的:优化气相色谱法测定酱油中对羟基苯甲酸酯类含量的分析方法。试样先后经饱和氯化钠溶液洗涤,盐酸酸化,无水乙醚提取,碳酸氢钠溶液洗涤后浓缩近干,无水乙醇溶解的条件下以外标法定量,通过5种不同极性的色谱柱与柱温箱温度的系列变化进行测试,最终确定最佳分离柱为Inert Cap 1301,柱温箱的初始温度为90℃。结果:对羟基苯甲酸酯类的加标回收率在91%~103%之间,相对标准偏差在0.6%~0.8%之间,对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯与对羟基苯甲酸丁酯的方法检出限分别为0.528mg/kg、0.497mg/kg、0.473mg/kg与0.440mg/kg。结论:优化仪器分析方法后,测定酱油中对羟基苯甲酸酯类含量的灵敏度明显提高,分析时间明显缩短,加标回收良好,这有利于提高检测分析效率,减小分析时间成本。

Object:To optimize the instrumental analysis method for the determination of parabens in soy sauce by gas chromatography.The sample was washed successively with saturated sodium chloride solution,acidified by hydrochloric acid,extracted by anhydrous ether,washed by sodium bicarbonate solution,concentrated and dried,and dissolved under the condition of absolute ethanol,and passed through 5 different polar columns.The series of changes in the temperature of the column oven were tested to determine the optimum separation column for the Inert Cap 1301 and the initial temperature of the column oven was 90℃.Results:The recoveries of parabens ranged from 91% to 103%,and the relative standard deviations ranged from 0.6% to 0.8%.The detection limits of methyl p-hydroxy benzoate,ethyl p-hydroxy benzoate,propyl p-hydroxy benzoate and butyl p-hydroxy benzoate were 0.528mg/kg,0.497mg/kg, 0.473mg/kg and 0.440mg/kg,respectively.Conclusion:After optimizing the instrumental analysis method,the sensitivity of determining the content of parabens in soy sauce is obviously improved,the analysis time is shortened obviously,and the standard addition recovery is good,which is beneficial to improve the efficiency of detection and analysis and reduce the analysis time cost.