高效液相色谱法同时测定食品中的苯甲酸、山梨酸、脱氢乙酸及糖精钠

目的:采用0.3%盐酸乙醇提取,低温下沉淀蛋白质,水定容离心过滤的前处理方法,高效液相色谱法同时测定苯甲酸、山梨酸、脱氢乙酸及糖精钠。方法:色谱柱DIONEX Acclaim120 C18(4.6×250 mm,5μm),甲醇-0.02 mol/L磷酸氢二钾溶液pH 7.0(10∶90)为流动相,流速:1.0 ml/min,检测波长:230 nm(苯甲酸、山梨酸、糖精钠)和293 nm(脱氢乙酸)。结果:苯甲酸、山梨酸、脱氢乙酸及糖精钠在0.1μg/ml～20μg/ml浓度范围内线性关系良好(r>0.9999),检出限小于0.4 mg/kg,其加标回收率在92.6%～105.4%之间,重复测定的RSD≤2.0%。结论:该方法操作简单,灵敏度高,准确性好,可应用于大批量样品的快速检测。

Simultaneous determination of benzoic acid,sorbic acid,dehydroacetic acid and sodium saccharin in food by HPLC

Objective:To establish a method for determination of benzoic acid,sorbic acid,dehydroacetic acid and sodium saccharin by HPLC.The preparation included extracting by 0.3% hydrochloric acid in ethanol,precipitating protein at low temperature and centrifuging and filtrating after constant volume with water.Methods: Column: DIONEX Acclaim 120 C18(4.6×250 mm,5 μm),Mobile phase: CH3OH–0.02 mol/L K2HPO4 pH 7.0(10∶ 90).Flow rate: 1.0 ml/min.Detection wavelength: 230 nm(benzoic acid,sorbic acid,sodium saccharin),293 nm(dehydroacetic acid).Results: Benzoic acid,sorbic acid,dehydroacetic acid and sodium saccharin showed good linearity(r>0.9999) in the range of 0.1 μg/ml～20 μg/ml.The detection limit was 0.4 mg/kg.The recoveries were between 92.6%～105.4%,the RSDs were less than 2.0%.Conclusion: This method is simple,accurate and reliable,which can be used for the determination of a large number of samples.