全自动固相萃取-高效液相色谱法检测胶基糖果中合成色素及铝色淀

Determination of synthetic pigments and aluminum-colored lakes in colloidal confectionery by fully automatic solid phase extraction-liquid chromatography

中文关键词:  胶基糖果  合成色素  铝色淀  高效液相色谱法  全自动固相萃取

英文关键词:colloidal confectionery  synthetic pigments  aluminum-colored lakes  high performance liquid chromatography  fully automatic solid phase extraction

中文摘要:

      目的 应用聚酰胺(polyamide, PA)净化技术建立胶基糖果中10种人工合成色素及其中8种铝色淀的全自动固相萃取-高效液相色谱法(high performance liquid chromatography, HPLC)。方法 样品经提取溶剂乙醇-2%氨水-水(4:2:4, V:V:V)超声提取, 离心, 经正己烷除脂, 除去乙醇和氨后, 以PA固相萃取小柱净化, 经Agilient Eclipse XDB-C18色谱柱分离, 以甲醇?0.02 mol/L乙酸铵溶液为流动相进行梯度洗脱, 二极管阵列检测器, 外标法定量。结果 在0.2~10.0 μg/mL质量浓度范围内各组分线性关系良好, 相关系数r2大于0.9999。游离色素平均回收率为85.1%~102.6%, 铝色淀平均回收率为78.9%~101.3%, 相对标准偏差为0.8%~5.9%。检出限除亮蓝为0.2 mg/kg, 其余均为0.5 mg/kg。结论 该方法有简单便捷、重复性好、准确度和灵敏度较高等特点, 适用于胶基糖果中合成色素及其铝色淀的测定。

英文摘要:

      Objective To establish an fully automatic solid phase extraction-high performance liquid chromatography (HPLC) method for the determination of 10 kinds of synthetic pigments and 8 kinds of aluminum-colored lakes in colloidal confectionery using polyamide (PA) purification technology. Methods The samples were extracted by ultrasonic solvent ethanol-2% ammonia-water (4:2:4, V:V:V), after centrifugation and lipid removal with hexane, removing ethanol and ammonia, purified by PA solidphase extraction column, separated by Agilient Eclipse XDB-C18 column, eluted with a gradient of methanol?0.02 mol/L ammonium acetate solution as the mobile phase, then detected by diode array detector, and quantitated by external standard method. Results The linear relationship of each component was good in the range of 0.2?10.0 μg/mL, the correlation coefficients were greater than 0.9999. The average recoveries of free pigments and aluminum-colored lakes were 85.1%?102.6%, 78.9%?101.3%, respectively. The relative standard deviations were 0.8%?5.9%. The limits of detection were 0.5 mg/kg except for bright blue, which was 0.2 mg/kg. Conclusion The method has the advantages of simple, convenient, good repeatability, high accuracy and sensitivity, and is suitable for the determination of synthetic colorants and aluminum-colored lakes in colloidal confectionery.