高效液相色谱法同时测定饮料中的苯甲酸、山梨酸、脱氢乙酸和糖精钠

Simultaneous Determination of Benzoic Acid in Beverages by HPLC Sorbic Acid,Dehydroacetic Acid and Saccharin Sodium

目的:建立高效液相色谱法(High Performance Liquid Chromatography,HPLC)同时测定饮料中的苯甲酸、山梨酸、脱氢乙酸和糖精钠的分析方法。方法:采用HPLC测定,色谱柱为ACE Excel 5 C18(4.6 mm×250 mm,5μm),流速为1.0 mL·min^(-1),波长为230 nm,流动相为20 mmoL·L^(-1)乙酸铵(pH7.5)∶甲醇(95∶5),用水提取样品并定容至25 mL过滤进样。结果:被测物苯甲酸、山梨酸、脱氢乙酸和糖精钠均能得到较好的分离,空白溶剂无干扰;方法线性范围为0~100 mg·L^(-1),相关系数均为0.9999以上,线性关系均良好;平均回收率为95.39%~99.96%,相对标准偏差(RSD)为0.20%~0.73%,苯甲酸、山梨酸、脱氢乙酸和糖精钠检出限为0.39~0.95 mg·kg^(-1);苯甲酸、山梨酸、脱氢乙酸和糖精钠定量限为1.30~3.16 mg·kg^(-1)。结论:高效液相色谱法操作简单,前处理时间短,分离度好,数据准确,重复性好,适用于饮料中苯甲酸、山梨酸、脱氢乙酸和糖精钠的同时检测。

Objective:To establish a method for the simultaneous determination of benzoic acid,sorbic acid,dehydroacetic acid and saccharin sodium in beverages by high performance liquid chromatography(HPLC).Methods:HPLC was used to determine the content,the chromatographic column was ACE Excel 5 C18(4.6 mm×250 mm,5μm).The mobile phase was 20 mmol·L^(-1) ammonium acetate(pH7.5)∶methanol(95∶5).The sample was extracted with water and diluted to 25 mL.Results:benzoic acid,sorbic acid,dehydroacetic acid and saccharin sodium could be separated well without interference of blank solvent;The linear range of the method was 0~100 mg·L^(-1),and the correlation coefficients were above 0.9999;The average recoveries ranged from 95.39%~99.96%,and the relative standard deviation(RSD)ranged from 0.20%~0.73%.The detection limits of benzoic acid,sorbic acid,dehydroacetic acid and saccharin sodium were 0.39~0.95 mg·kg^(-1);The loqs of benzoic acid,sorbic acid,dehydroacetic acid and saccharin sodium were 1.30~3.16 mg·kg^(-1).Conclusion:HPLC has the advantages of simple operation,short pretreatment time,good resolution,accurate data and good repeatability,which is suitable for the simultaneous determination of benzoic acid,sorbic acid,dehydroacetic acid and saccharin sodium in beverages.