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目的建立固相萃取-超高效液相色谱法同时测定蜜饯中柠檬黄、新红、胭脂红、苋菜红、靛蓝、日落黄、诱惑红、亮蓝、赤藓红9种合成色素。方法样品采用乙醇氨提取,阴离子固相萃取小柱净化,经ZORBAX SB-C_(18)色谱柱分离,甲醇和0.02 mol/L乙酸铵为流动相梯度洗脱,流速0.4 m L/min。采用二极管阵列检测器,采集254 nm(0~8.0 min)、300 nm(8.0~9.5 min)、254 nm(9.5~18.0 min)色谱合成图进行外标法定量,并通过与对照品的光谱比对进行确证。结果 9种合成色素在18 min内可有效分离,在0.4~40μg/m L的线性范围内相关系数均为0.9999,平均回收率为80.1%~98.6%,相对标准偏差为1.8%~5.2%,检测限为1~2 ng。结论该方法前处理简单、检测快速、回收率满意且重复性好,可作为蜜饯中9种合成色素的检测方法。
OBJECTIVE To establish a solid phase extraction coupled with ultra performance liquid chromatography (HPLC) for the simultaneous determination of nine synthetic pigments, lemon yellow, red, carmine, amaranth, indigo, sunset yellow, seductive red, brilliant blue and erythrosine in candied fruit. Methods The samples were eluted with ethanol ammonia and cleaned up with anion solid phase extraction cartridges. The residue was separated on a ZORBAX SB-C 18 column. The mobile phase consisted of methanol and 0.02 mol / L ammonium acetate. The flow rate was 0.4 m L / min. The diode array detector was used to collect the chromatograms of 254 nm (0 ~ 8.0 min), 300 nm (8.0 ~ 9.5 min) and 254 nm (9.5 ~ 18.0 min) To confirm. Results Nine synthetic pigments were effectively separated within 18 min. The correlation coefficient was 0.9999 in the linear range of 0.4-40 μg / mL. The average recoveries ranged from 80.1% to 98.6% with relative standard deviations of 1.8% -5.2% The detection limit is 1 ~ 2 ng. Conclusion This method is simple, rapid detection, satisfactory recovery and good reproducibility, and can be used as a detection method for nine kinds of synthetic pigment in candied fruit.