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    超高效液相色谱法测定饮料中的25种常见和新型食品添加剂

    Determination of 25 Common and New Food Additives in Beverages by Ultra-High Performance Liquid Chromatography

    • 摘要: 建立了超高效液相色谱法(UHPLC)同时测定饮料中25种常见和新型食品添加剂(专利蓝V和爱德万甜)的方法。取2.5 g样品,用50%(体积分数)甲醇溶液定容至25 mL,涡旋振荡2 min,超声提取20 min,过0.45 μm聚四氟乙烯(PTFE)滤膜,滤液供UHPLC分析。在ACQUITY UPLC® HSS T3色谱柱上以不同体积比的甲醇-0.02 mol·L-1乙酸铵溶液的混合溶液为流动相进行梯度洗脱,分离得到的食品添加剂用光电二极管阵列检测器在多波长下检测。结果显示:25种食品添加剂的质量浓度均在一定范围内与其对应的色谱峰面积呈线性关系,检出限(3S/N)为0.2~3.0 mg·kg-1;对实际样品进行加标回收试验,所得回收率为82.1%~111%,测定值的相对标准偏差(n=6)为0.19%~3.1%。方法用于7种果蔬汁饮料和3种茶饮料的分析,在3个茶饮料样品中均检出了咖啡因(95.3,98.4,124.9 mg·kg-1),在1个果蔬汁饮料样品中检出了安赛蜜(20.2 mg·kg-1),2个果蔬汁饮料样品检出了山梨酸(15.8,18.9 mg·kg-1)。

       

      Abstract: A method for determination of 25 common and new food additives (patent blue V and advantame) in beverages by UHPLC. The sample (2.5 g) was taken and its volume was made up to 25 mL with 50% (volume fraction) methanol solution. The mixed solution was shaken for 2 min by vortex, extracted by ultrasound for 20 min, and passed through a 0.45 μm PTFE filtering membrane. The filtrate obtained was analyzed by UHPLC. Mixed solutions composed of methanol and 0.02 mol·L-1 ammonium acetate solution with various volume ratios were used as mobile phase for gradient elution on a ACQUITY UPLC® HSS T3 chromatographic column. The food additives separated were detected by photodiode array detector at multi-wavelengths. The results showed that linear relationships between mass concentrations of 25 food additives and their corresponding peak areas were kept in definite ranges, with detection limits (3S/N) in the range of 0.2-3.0 mg·kg-1. Test for recovery was made on actual samples by standard addition method, giving values of recovery in the range of 82.1%-111%, and RSDs (n=6) of the determined values ranged from 0.19% to 3.1%. The proposed method was applied to analysis of 7 fruit and vegetable beverages and 3 tea beverages, caffeine (95.3, 98.4, 124.9 mg·kg-1) was detected in 3 tea beverages, and acesulfame (20.2 mg·kg-1) was detected in 1 fruit and vegetable beverage, and sorbic acid (15.8, 18.9 mg·kg-1) was detected in 2 fruit and vegetable beverages.

       

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