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目的建立同时测定辣椒制品和豆制品中非法添加的苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅲ、苏丹红Ⅳ、苏丹红7B、二甲基黄以及二乙基黄7种常见偶氮染料的超快速液相色谱-串联质谱法。方法样品经酸性乙腈提取、通过比较OasisPRi ME HLB、HLB以及MAX 3种固相萃取柱的净化效果,最终选择PRi ME HLB作为实验用柱。提取液用PRi ME HLB固相萃取柱净化后,以水/乙腈(内含0.1%甲酸)为流动相,经Agilent Eclipse Plus C_(18)(100 mm×2.1 mm,1.8μm)色谱柱分离洗脱,电喷雾正离子MRM模式检测。结果 7种待测化合物在各自检测范围内均具有良好的线性关系(r>0.999),方法的最低定量检出限为0.02μg/kg~0.1μg/kg,在辣椒酱和豆干中的平均回收率分别为78.2%~91.9%和82.7%~93.9%,精密度分别为1.69%~4.82%和1.82%~4.09%。结论本方法分析速度快、重现性好、准确、灵敏,适用于辣椒制品(干辣椒和辣椒酱)和豆制品(豆干和腐竹)中7种偶氮染料的确证检测。
OBJECTIVE To establish a method for the simultaneous determination of seven common azo dyes such as Sudan I, Sudan II, Sudan III, Sudan IV, Sudan 7B, dimethyl yellow and diethyl yellow illegally added to pepper products and soy products Fast liquid chromatography - tandem mass spectrometry. Methods The samples were extracted with acidic acetonitrile. The purification results of the HLB, HLB, and MAX columns were compared. Finally, PRi ME HLB was selected as the experimental column. The extract was purified with a PRi ME HLB solid phase extraction cartridge and separated on a Agilent Eclipse Plus C 18 (100 mm × 2.1 mm, 1.8 μm) column using water / acetonitrile (0.1% formic acid as mobile phase) Off, electrospray positive ion MRM mode detection. Results The seven compounds tested had a good linear relationship (r> 0.999) within the limits of detection. The detection limit of the method was 0.02μg / kg ~ 0.1μg / kg. The average The recoveries were 78.2% -91.9% and 82.7% -93.9%, respectively, with the precision of 1.69% -4.82% and 1.82% -4.09%, respectively. Conclusion The method is rapid, reproducible, accurate and sensitive. It is suitable for the confirmation of seven azo dyes in chili products (dried chili and chili sauce) and bean products (dried bean and dried bean curd).