复杂食品基质中12种人工色素高通量检测技术研究

High throughput detection of 12 kinds of artificial pigments in complex food substrates

目的 建立高通量快速检测多种复杂食品基质中12种人工色素(柠檬黄、日落黄、新红、苋菜红、胭脂红、亮蓝、诱惑红、赤藓红、酸性红、喹啉黄、专利蓝V和胭脂红SX)的分析方法。方法 对比优化多种前处理方式,确定样品使用无水乙醇-乙腈-氨水-水溶液提取,混合弱阴离子固相萃取柱净化, XDB-C_(18)色谱柱(250 mm×4.6 mm, 5μm)分离,以0.02 mol/L乙酸铵溶液与甲醇为流动相进行梯度洗脱,使用高效液相色谱-二极管阵列检测器(high performance liquid chromatography-photodiode array detector, HPLC-PDA)在430、507和630nm紫外波长下进行定量分析。对于假阳性样品,采用高效液相色谱-串联质谱法确证。结果 12种人工色素在0.02~40.00μg/mL范围内线性相关系数均大于0.9999,检出限为0.023~0.079mg/kg,加标回收率为72.4%~99.7%,相对标准偏差均小于8%。结论 该方法具有前处理简单、快速,回收率好、分析结果稳定的特点,可用于大批量肉制品、胶囊类保健食品、糕点、含胶质类糖果等多种复杂食品基质中的12种人工色素的快速筛查和含量测定。

Objective To establish high throughput methods for the rapid detection of detection of 12 kinds of artificial pigments(tartrazine,sunset yellow,new red,amaranth,ponceau 4RC,brilliant blue FCF,allura red AC,erythrosine B,azorubin,quinoline yellow,patent blue V and ponceau SX)in a variety of complex food substrates.Methods Various pre-treatment methods were compared and optimized.It was determined that the sample was extracted with by anhydrous ethanol-acetonitrile-ammonian-aqueous solution,purified by solid phase extraction column,separated by XDB-C_(18) column(250 mm×4.6 mm,5μm),and gradient eluted with 0.02 mol/L ammonium acetate solution and methanol as mobile phase,and high performance liquid chromatography-diode array detector(HPLC-PDA)was used for quantitative analysis at 430,507 and 630 nm ultraviolet wavelengths.The false positive samples were qualitatively screened by high performance liquid chromatography-tandem mass spectrometry.Results The linear correlation coefficients of the 12 kinds of artificial pigments were all greater than 0.9999 in the range of 0.02‒40.00μg/mL,the limits of detection were 0.023‒0.079 mg/kg,the recoveries were 72.4%‒99.7%,and the relative standard deviations were<8%.Conclusion The method has the advantages of simple,rapid pretreatment,good recovery and stable analysis results.It can be used for rapid screening and content determination of 12 kinds of artificial pigments in a large quantities of multiple complex substrates foods such as large-scale meat products,capsule health food,pastries,gelatinous candy,etc..