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目的探讨用全自动固相萃取-HPLC法检测食品中7种合成色素。方法样液在全自动固相萃取仪上,经PA(聚酰胺粉1 g/6ml)或PWAX(弱阴离子150 mg/6ml)SPE小柱净化,以甲醇和乙酸铵为流动相,在C18色谱柱上分离,梯度洗脱,紫外254 nm及可见625 nm波长检测,外标法定量。结果在0.2μg/ml~20μg/ml浓度范围内相关系数0.9994~0.9999,最低检出限0.005μg/ml~0.01μg/ml。PA(聚酰胺粉1g/6ml)SPE小柱净化,回收率86.9%~104.5%、RSD为1.3%~7.5%。PWAX(弱阴离子150 mg/6ml)SPE小柱净化,回收率89.3%~103.6%、RSD为0.5%~4.7%。结论样品前处理使用自动化操作,色素吸附效果好、大大减少试剂用量、简单、方便,7种色素分离度好、回收率满意,适合大批量样品检测。
Objective To investigate the detection of seven kinds of synthetic pigments in foods by automatic solid-phase extraction-HPLC. Methods The sample solution was purified on a SPE (1 g / 6 ml PA) or PWAX (weak anion 150 mg / 6 ml) SPE cartridges using methanol and ammonium acetate as mobile phases and C18 chromatography Column separation, gradient elution, UV 254 nm and visible 625 nm wavelength detection, external standard quantitative. Results The correlation coefficients ranged from 0.9994 to 0.9999 in the range of 0.2μg / ml to 20μg / ml with the detection limit of 0.005μg / ml to 0.01μg / ml. PA (polyamide powder 1g / 6ml) SPE column purification, the recovery rate of 86.9% to 104.5%, RSD of 1.3% to 7.5%. PWAX (weak anion 150 mg / 6 ml) SPE cartridges. The recoveries ranged from 89.3% to 103.6% with RSD from 0.5% to 4.7%. Conclusion The sample pretreatment using automated operation, pigment adsorption effect is good, greatly reducing the reagent dosage, simple and convenient, good separation of seven kinds of pigments, satisfactory recovery rate, suitable for large sample testing.