固相萃取-高效液相色谱法同时测定食品中4种合成色素

Simultaneous determination of four pigments in food by solid phase extraction combined with high performance liquid chromatography

以可代替使用的水溶性合成色素-亮黑BN、固绿FCF、酸性红、酸性黄36为研究对象,建立了高效液相色谱同时测定食品中4种合成色素的方法。样品通过WAX固相萃取柱富集净化,10%氨化甲醇洗脱,采用C18色谱柱分离,以甲醇和10 mmol/L乙酸铵水溶液作为流动相梯度洗脱,外标法定量。通过固相萃取柱净化后,杂质对待测物的干扰明显降低,优化色谱条件下,4种色素在0.10~10.0 mg/L质量浓度范围内,线性良好,相关系数(r)≥0.9995。方法回收率为92.6%~101.8%,相对标准偏差(RSD)≤5.4%,方法检出限为0.01~0.04 mg/kg。该方法灵敏度高,准确可靠,适合食品中亮黑BN、固绿FCF、酸性红、酸性黄36的同时测定。

An analytical method for the simultaneous determination of four pigments including brilliant black BN,fast green FCF,azorubine and acid yellow 36 in food was developed by solid phased extraction(SPE)-high performance liquid chromatography.The samples were purified and enriched with WAX cartridge with 10%ammoniated methanol as elution,then the analytes were separated by C18 column using a mobile phase consisting of methanol and 10 mmol/L ammonium acetate in gradient mode.Clean extraction was achieved using SPE operation,and the interferences were well excluded.Under optimizing chromatographic conditions,the four pigments showed good linearity in the range of 0.10~10.0 mg/L(r≥0.9995).The recoveries were92.6%-101.8%,the relative standard deviations(RSDs)were less than 5.4%,and the detection limits were0.01-0.04 mg/kg.The method was accurate and sensitive,which was suitable for the simultaneous detection of brilliant black BN,fast green FCF,azorubine and acid yellow 36 in food.