| 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-C18色谱柱(250 mm×4.6 mm, 5 μm)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630 nm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0.02~40.00 μg/mL范围内线性相关系数均大于0.9999, 检出限为0.023~0.079 mg/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-C18 column (250 mm×4.6 mm, 5 μm), 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?40.00 μg/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.. |
