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目的建立固相萃取-高效液相色谱法测定多种类食品中靛蓝、亮蓝的检测方法。方法采用固相萃取技术,用乙腈水溶液提取样品中色素并经WAX小柱净化,以甲醇-0.02 mol/L乙酸铵溶液作为流动相梯度洗脱,经Waters Symmetry C_(18)(5μm,4.6 mm×250 mm)色谱柱分离,运用高效液相色谱-二极管阵列检测器(HPLC-PDA)检测。结果该方法靛蓝、亮蓝在0.50~20.00μg/m L范围内有较好的线性关系,均r>0.999;靛蓝和亮蓝的方法检出限分别为0.04和0.02 mg/kg;样品加标平均回收率为81.8%~101.1%,相对标准偏差为2.1%~4.9%(n=6)。结论该方法具有较高的选择性和灵敏度,回收率和重现性良好,可用于GB 2760—2014食品分类系统中多种类食品中靛蓝、亮蓝含量的分析。
Objective To establish a method for the determination of indigo and brilliant blue in many kinds of food by solid phase extraction and high performance liquid chromatography. Methods Solid phase extraction (SPE) was used to extract the pigment from the sample with aqueous acetonitrile and eluted with WAX cartridge. The mobile phase was eluted with methanol - 0.02 mol / L ammonium acetate solution. The mobile phase was eluted with Waters Symmetry C18 (5 μm, 4.6 mm × 250 mm) column and detected by HPLC-PDA (High Performance Liquid Chromatography-Diode Array Detector). Results The method showed a good linear relationship between indigo and brilliant blue in the range of 0.50 ~ 20.00 μg / m L, all of which were r> 0.999. The detection limits of indigo and brilliant blue were 0.04 and 0.02 mg / kg, respectively. The average recoveries ranged from 81.8% to 101.1% with relative standard deviations of 2.1% to 4.9% (n = 6). Conclusion The method has high selectivity and sensitivity, good recovery and reproducibility, and can be used for the analysis of indigo and brilliant blue content in a variety of foods GB 2760-2014 food classification system.