食品与机械2024,Vol.40Issue(3) :82-88,94.DOI:10.13652/j.spjx.1003.5788.2023.80583

全自动固相萃取—高效液相色谱法测定现制饮料中7种合成着色剂

Determination of 7 synthetic colorants in freshly prepared beverages by high performance liquid chromatography dual wavelength method with automatic solid phase extraction

姚誉阳 徐曼 潘春燕 缪雄 薛强
食品与机械2024,Vol.40Issue(3) :82-88,94.DOI:10.13652/j.spjx.1003.5788.2023.80583

全自动固相萃取—高效液相色谱法测定现制饮料中7种合成着色剂

Determination of 7 synthetic colorants in freshly prepared beverages by high performance liquid chromatography dual wavelength method with automatic solid phase extraction

姚誉阳 1徐曼 2潘春燕 1缪雄 3薛强1
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作者信息

  • 1. 无锡市疾病预防控制中心[南京医科大学附属无锡疾病预防控制中心],江苏无锡 214023
  • 2. 新疆克拉玛依市疾病预防控制中心,新疆克拉玛依 834000
  • 3. 无锡市食品安全检验检测中心,江苏无锡 214142;国家市场监管技术创新中心[特殊食品],江苏无锡 214142
  • 折叠

摘要

目的:建立一种全自动固相萃取—高效液相色谱双波长法测定现制饮料中7种合成着色剂的方法.方法:样品经纯水提取2次,离心后,合并上清液,调节pH至3~4.利用全自动固相萃取装置活化Poly-sery色素专用固相萃取小柱,并上样、淋洗、洗脱.洗脱液氮吹浓缩至200 μL,用50%流动相A+50%流动相B混合液定容至1.0 mL.色谱柱采用C18柱,流动相为20 mmol/L乙酸铵—甲醇,梯度洗脱,流速1.0 mL/min,进样量10μL,检测波长254,628 nm.结果:各物质在0.5~50.0 μg/mL范围内相关系数均大于0.999 9,方法检出限为 0.023~0.179 mg/kg,定量限为 0.078~0.598 mg/kg,加标回收率为92.4%~96.8%,相对标准偏差(RSD)为1.2%~4.2%.结论:该方法试剂使用量小,操作步骤简便,自动化程度高,回收率高,重复性好,适合于批量样品测定.

Abstract

Objective:A method for the determination of 7 synthetic colorants in freshly prepared beverages by high performance liquid chromatography dual(HPLC)wavelength method with automatic solid phase extraction was established.Methods:Extraction conditions:The sample was extracted 2 times with pure water,and then the supernatant combined after centrifugation.The pH of the supernatant was adjusted to 3~4.After activation by an automatic solid-phase extraction device,loading,rinsing,and elution of the sample were carried out on the Poly-sery synthetic colorant solid-phase extraction column.The eluent was concentrated to 200 μL by nitrogen blowing,and then fixed to 1.0 mL with 50%mobile phase A+50%mobile phase B.Instrument conditions:The column was C18 column.The mobile phase was 20 mmol/L ammonium acetate-methanol,gradient elution.The flow rate was 1.0 mL/min.The injection volume was 10 μL.The detection wavelength were 254 nm and 628 nm.Results:The correlation coefficient of each substance in the range of 0.5~50 μg/mL was greater than 0.999 9,the detection limit of the method was 0.023~0.179 mg/kg,the quantitative limit was 0.078~0.598 mg/kg,the standard recovery was 92.4%~96.8%,and the relative standard deviation(RSD)was 1.2%~4.2%.Conclusion:This method has low consumption of toxic reagents,simple operation steps,high degree of automation,good recovery and repeatability,and it is suitable for the determination of large quantities of samples.

关键词

全自动固相萃取/高效液相色谱法/现制饮料/合成着色剂

Key words

automatic solid phase extraction/high performance liquid chromatography(HPLC)/freshly prepared beverages/synthetic colorant

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基金项目

无锡市卫生健康委重点学科建设项目(LCZX2021006)

新疆维吾尔自治区卫生健康青科项目(WJWY-202307)

出版年

2024
食品与机械
长沙理工大学

食品与机械

CSTPCD北大核心
影响因子:0.89
ISSN:1003-5788
参考文献量15
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