冰淇淋中着色剂检测前处理方法的优化

Optimization of treatment method for colorants pretest in ice cream

建立了一种测定复杂基质样品冰淇淋中柠檬黄、苋菜红、胭脂红、日落黄、亮蓝5种合成着色剂的高效液相色谱分析方法。采用甲醇作为提取剂,将着色剂解吸为溶液状态,使用聚酰胺小柱固相萃取法(SPE)净化,HPLC测定。结果表明,相对于GB 5009.35-2016的处理方式,该方法节省前处理时间、节约试剂、净化过程清晰明了,消除了提取不充分及抽滤困难的情况,5种着色剂组分的检出限分别为0.026、0.025、0.029、0.026、0.18mg/kg,在10 mg/kg的加标水平下,回收率为83.1%、84.4%、79.7%、89.0%、89.4%,较标准方法提高10%。拓展了国标对合成着色剂(色素)测定的适用范围,针对不同组成的冰淇淋和雪糕样品给予了具体的前处理方案,该方法针对性强,为冰淇淋中超量或违法添加色素的监督检验提供了科学优质的途径,具有较高的实际应用价值。

In this experiment,a high performance liquid chromatographic method for the determination of lemon yellow,amaranth,carmine,sunset yellow and brilliant blue in ice cream with complex matrix was established. Methanol was used to desorb the colorants into solution,SPE method was used in purification,and the extractive was tested by HPLC. The results showed that compared with the treatment method GB 5009.35-2016,this method cost less time and reagents with simple purification process. The problem of insufficient extraction to different types of ice cream was solved,and the use of SPE method eliminated the difficulty of filtration. The LOD of five colorants was 0.026,0.025,0.029,0.026 and 0.18 mg/kg. The recovery rate of the five colorants at the spiked level of 10 mg/kg was 83.1%,84.4%,79.7%,89.0% and 89.4%,which is higher than that of the GB method by 10%. The scope of the determination of synthetic colorants（pigments）was expanded,and specific pretreatment scheme was given for samples such as ice cream and popsicle with different compositions. This method has strong pertinence and is a high quality scientific method with high practical application value to identify excessively or illegally added colorants in ice cream.