高效液相色谱法同时测定泡椒凤爪中的苯甲酸和山梨酸

目的:建立同时测定泡椒凤爪中的苯甲酸、山梨酸的高效液相色谱(HPLC)分析方法。方法:样品经搅碎、碱水超声提取、甲醇沉淀蛋白、过滤后进样测定。色谱条件:色谱柱为dC18柱(5μm,4.6×150 mm),流动相为甲醇-乙酸铵(0.02 mol/L)(20∶80);流速为1 ml/min;柱温为40℃;检测波长为254 nm。结果:苯甲酸、山梨酸在0 mg/ml～0.10 mg/ml浓度范围内,线性关系良好,相关系数(r)分别为0.9992和0.9994;苯甲酸的相对标准差(RSD)为0.82%～5.5%、山梨酸为0.57%～4.0%;苯甲酸的加标回收率为92.0%～99.6%,山梨酸为91.3%～104.0%。结论:本方法快速、准确,可有效消除干扰,精密度、准确性均满足检测要求,适合于泡椒凤爪中苯甲酸和山梨酸的同时测定。

Simultaneous determination of benzoic acid and sorbic acid in pickled chicken paws by high performance liquid chromatography

Objective:To develop a method for the simultaneous determination of benzoic acid and sorbic acid in pickled chicken paws by high performance liquid chromatography(HPLC).Methods: The chopped sample was extracted with alkaline water,and then the protein in sample solution was precipitated with methanol in neutral condition and finally the sample solution was filtrated and injected for determination.The chromatographic conditions: Waters dC18 column(4.6×150 mm,5 μm) was used for separation,the mobile phase was methanol-ammonium acetate(20∶ 80) at a flow rate of 1 ml/min and detection wavelength was set at 254 nm.The column temperature was 40℃.Results: The correlation coefficients for these two preservatives were all greater than 0.999 with RSD<6%.The recoveries were 92.0%~99.6% and 91.3%~104.0% for benzoic acid and sorbic acid respectively.Conclusion: The method is simple,rapid,accurate and suitable for the simultaneous determination of the benzoic acid and sorbic acid in pickled chicken paws.