高效液相色谱法同时测定碳酸饮料中13种食品添加剂

Simultaneous determination of 13 kinds of food additives in sodas by high performance liquid chromatography

目的采用高效液相色谱法建立同时检测碳酸饮料中防腐剂、抗氧化剂、稳定剂（苯甲酸、山梨酸）、甜味剂（安赛蜜、糖精钠）和9种着色剂（柠檬黄、新红、苋菜红、靛蓝、胭脂红、日落黄、诱惑红、亮蓝和赤鲜红）的分析方法。方法将待测饮料样品经水稀释到合适的浓度,离心过滤后,以10 mmol/L醋酸铵溶液-10mmol/L醋酸铵甲醇溶液作为流动相在ZORBAX SB-Aq（3.0 mm×150 mm,3.5μm）色谱柱上梯度洗脱进行分离,检测波长为230、427、507、620 nm。以目标物的色谱保留时间和紫外光谱图与标准物质一致进行定性分析。以色谱峰的峰面积用标准曲线外标法进行定量。结果在优化条件下,各目标物的线性范围为0.1-100 mg/L,相关系数均大于0.999。13种食品添加剂的定量限为0.5-1.5 mg/kg。在低、中、高3个水平下,各目标物的回收率在90%-110%之间,相对标准偏差（RSD）均低于10%。结论该方法准确、简便、灵敏、可靠,可用于碳酸饮料中此13种食品添加剂的同时定量测定。

Objective To establish a method for the simultaneous determination of preservatives（benzoic acid and sorbic acid）, sweet agents（acesulfame and saccharin sodium dehydrate） and colorants（hydrazine yellow, new red, naphthol red, acid blue 74, carmine, sunset yellow, allura red, brilliant blue and acid red 51） in sodas by high performance liquid chromatographic（HPLC）. Methods Sodas samples were diluted to the right concentration by 10 mmol/L ammonium acetate. After filtered, the extract was separated on an ZORBAX SB-Aq column（3.0 mm×150 mm, 3.5 μm） using a gradient elution program with mobile phase of 10 mmol/L ammonium acetate- 10 mmol/L ammonium acetate methanol solution. Detection wavelengths were set at 230, 427, 507 and 620 nm, respectively. The qualitative analysis was based on chromatographic retention time and UV spectrum, and the quantitative analysis was performed by the standard curve method of peak area. Results The linear ranges of 13 analytes were in the range of 0.1-100 mg/L, with correlation coefficients more than 0.999. The limits of quantiation（LOQs） were in the range of 0.5-1.5 mg/kg. The average recoveries at three spiked levels ranged from 90%-110% with RSDs less than 10%. Conclusion This method is accurate, simple, sensitive and reliable, and can be used for the simultaneous determination of 13 kinds of food additives in sodas.