高压液相色谱法快速测定饮料中的五种食品添加剂

Rapid determination of five food additives in soft drinks by high pressure liquid chromatography

中文关键词:  高压液相色谱法  快速分析  甜味剂  防腐剂  饮料

英文关键词:high pressure liquid chromatography  rapid analysis  sweeteners  preservatives  soft drinks

中文摘要:

      目的 建立一种高压液相色谱方法同时检测饮料制品中3种甜味剂(安赛蜜、糖精钠、阿斯巴甜)和2种防腐剂(苯甲酸、山梨酸)。方法 样品采用起始流动相稀释后直接过膜分析, 色谱分离在极性修饰XAqua C18色谱柱上进行, 流动相采用50 mmol/L pH 4.5 KH2PO4和乙腈, 梯度模式洗脱, 流速2 mL/min, 柱温40 ℃, 6 min内即可完成一次分离分析, 加上4 min梯度平衡时间, 10 min内即可完成平衡及分离。结果 5种食品添加剂在0.5~50 mg/L内线性关系良好, 相关系数r2均大于0.9999。在两种饮料基质中添加50、100、150 mg/kg 3个浓度水平, 方法回收率为96.48%~105.64%, 相对标准偏差为0.21%~5.39%; 以信噪比S/N =3计算, 方法检测限为0.02~0.08 mg/L。结论 建立的分析方法快速、准确, 可满足饮料中甜味剂和防腐剂的同时检测。

英文摘要:

      Objective To establish a high pressure liquid chromatography method for the simultaneous determination of 3 sweeteners (acesulfame-K, saccharin sodium, aspartame) and 2 preservatives (benzoic acid, sorbic acid) in soft drinks. Methods The samples were diluted with initial mobile phase and filtrated for liquid chromatographic analysis. The separation was performed on a polar-modified XAqua C18 column with 50 mmol/L pH 4.5 KH2PO4 and acetonitrile as mobile phase in gradient mode. The flow rate was set at 2 mL/min and column temperature was 40℃. The separation could be achieved within 6 min. And one sample could be analyzed within 10 min with the addition of 4 min equilibration time. Results Under the optimized chromatographic conditions, a good linearity was obtained in the range of 0.5~50 mg/L for the 5 food additives, with correlation coefficients (r2) all above 0.9999. For samples (carbonated and fruit juice beverage matrix) spiked with 50, 100 and 150 mg/kg of the 5 food additives, the recoveries and relative standard deviations (RSD) were 96.48%~105.64% and 0.21%~5.39%, respectively. The limits of detection (LOD) of the method calculated by signal to noise ratio (S/N) = 3:1 was 0.02~0.08 mg/L. Conclusion The developed analysis method was rapid and accurate, and could be used for the simultaneous determination of sweeteners and preservatives in soft drinks.