超高效液相色谱法同时测定含乳饮料中12种食品添加剂

Simultaneous determination of 12 kinds of food additives in milk-containing beverages by ultra performance liquid chromatography

目的建立超高效液相色谱法同时快速测定含乳饮料中3种甜味剂、7种防腐剂和2种酸味剂的检测方法。方法样品用水提取后,加入亚铁氢化钾和乙酸锌溶液沉淀蛋白质及其他杂质。以Waters XBridge BEHC18柱(100mm×2.1mm,i.d.1.7μm)为分离柱,甲醇-20mmol/L乙酸铵溶液为流动相梯度洗脱,流速为0.3 mL/min,采用二极管阵列检测器进行检测,检测波长为230 nm和210 nm。结果 12种目标物可以在6 min内达到较好的分离,在0.010～80μg/mL范围内呈良好的线性关系(r2≥0.9996),检出限为0.03～0.15 mg/kg,定量限0.10～0.50mg/kg,样品在3个加标水平(1、10和50mg/kg)的回收率为80.2%～99.7%,相对标准偏差为1.23%～4.70%。结论该方法操作简单,快速,适用于含乳饮料中12种食品添加剂的检测。

Objective To establish a method for simultaneous determination of 3 kinds of preservatives, 7 kinds of sweeteners and 2 kinds of acidulants in milk-containing beverage by ultra performance liquid chromatography(UPLC). Methods After the sample was extracted with water, ferrous potassium hydride and zinc acetate solution were added to precipitate proteins and other impurities, and then it was gradient eluted by a column of Waters XBridge BEH C18(100 mm×2.1 mm, i.d. 1.7 μm) with the mobile phase of methanol and 20 mmol/L ammonium acetate solution at a flow rate of 0.3 mL/min. Detection was performed using a diode array detector with detection wavelengths of 230 nm and 210 nm. Results The 12 kinds of food additives could be effectively separated within 6 min. In the range of 0.010-80 μg/mL, there was a good linear relationship(r2≥0.9996), the limit of detection was 0.03-0.15 mg/kg, and the limit of quantification was 0.10-0.50 mg/kg. The recoveries of samples at 3 levels(1, 10 and 50 mg/kg) were 80.2%-99.7% and the relative standard deviations(RSDs) were 1.23%-4.70%. Conclusion This method is rapid and convenient, which is suitable for the determination of 12 kinds of food additives in milk-containing beverages.