全自动固相萃取-液相色谱法同时测定饮料中的11种合成着色剂
Simultaneous determination of 11 kinds of synthetic colorants in beverages by automated solid-phase extraction-liquid chromatography
投稿时间:2025-02-12  修订日期:2025-04-11
DOI:
中文关键词:  全自动固相萃取法  高效液相色谱法  合成着色剂  饮料
英文关键词:fully-automatic solid phase extraction method  high-performance liquid chromatography  synthetic colorant  beverage
基金项目:
作者单位
李彪 阜阳市产品质量监督检验所 
张岩岩 国家再生有色金属橡塑材料产品质量监督检验中心(安徽) 
徐宏岩 阜阳市产品质量监督检验所 
AuthorInstitution
LI Biao Fuyang Institute of Product Quality Supervision & Inspection 
ZHANG YanYan National Recycled Nonferrous Metal Rubber & plastic materials Quality Supervision and Inspection Center (Anhui) 
XU Hong-Yan Fuyang Institute of Product Quality Supervision & Inspection 
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中文摘要:
      摘 要:目的 建立了全自动固相萃取和液相色谱联用同时测定饮料中11中合成作色剂含量的方法。方法 取2 g饮料试样,用氨水乙醇溶液提取,借助全自动固相萃取仪依次进行活化、上样、淋洗、洗脱、收集操作,氮吹复溶后采用液相色谱仪[二极管阵列多波长多通道同时检测,检测波长 415 nm (柠檬黄、喹啉黄),520 nm(新红、苋菜红、胭脂红、 日落黄、诱惑红、酸性 红和赤藓红),610 nm(靛蓝、亮蓝);流动相:A 为 20 mmol/L 乙酸铵溶液,B 为甲醇,流速1 ml/min梯度洗脱]上机测定。结果 在0.2~10.0 μg/mL质量浓度范围内,11种合成着色剂的浓度与峰面积呈现良好线性关系,线性相关系数均大于0.99,检出限符合GB 5009.35—2023《食品安全国家标准 食品中合成作色剂的测定》要求。标准加入法回收试验中,回收率处于92.5%~106%,测定值的相对标准偏差(n=6)均小于5.0%。将该方法应用于长三角食品类检测机构饮料中的胭脂红、日落黄能力验证,胭脂红含量为5.86 mg/kg,日落黄含量为4.31 mg/kg,其余合成着色剂均未检出。结论 该方法可实现前处理富集效果好、自动化程度高、操作简单、稳定性好、时间短、效率高、灵敏性好,准确度高、重现性好,适用于大批量饮料中合成着色剂的测定分析。
英文摘要:
      ABSTRACT: Objective A fully automated method for the simultaneous determination of 11 synthetic colorants in beverages by solid phase extraction and chromatography was established. Methods Take 2 g of beverage sample, extract it with ammonia ethanol solution, and perform operations such as activation, sample loading, washing eluting, and collection in turn with the help of a fully automatic solid phase extraction instrument. After nitrogen blowing and redissolution, the liquid chromatography instrument [diode multi-wavelength multi-channel simultaneous detection, detection wavelength 415 nm (Citrus Yellow, Quinoline Yellow), 520 nm (New Red Amaranth, Carmine, Sunset Yellow, Temptation Red, Acidic Red, and Red Algae), 610 nm (Indigo, Bright Blue mobile phase: A 20 mmol/L ammonium acetate solution, B methanol, flow rate 1 ml/min gradient elution] was used on-line determination. Results In the range of 0.2~10.0 μg/mL, the concentration of 11 synthetic colorants showed good linear relationship with peak area, and the linear correlation coefficients were all greater than 0.99, the limit of detection met the requirements of GB 500935—2023 "National Food Safety Standard for the Determination of Synthetic Colorants in Food". In the standard addition method recovery test, the recovery rate between 92.5% and 106%, and the relative standard deviation of the determination value (n=6) was less than 5.0% This method was applied to the ability verification of Sunset Yellow and Carmine in beverages in food testing institutions in the Yangtze River Delta. The content of Carmine was 586 mg/kg, and the content of Sunset Yellow was 4.31 mg/kg. The other synthetic colorants were not detected. Conclusions This method achieve good enrichment effect, high automation degree, simple operation, good stability, short time, high efficiency, good sensitivity, high accuracy, and good reproducibility, and is suitable the determination and analysis of synthetic colorants in a large number of beverages.
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