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目的以WAX固相萃取柱净化处理,建立豆制品中违禁添加色素碱性橙Ⅱ、碱性嫩黄O、酸性橙Ⅱ和罗丹明B的前处理方法。方法利用电喷雾离子源(ESI),碱性橙、碱性嫩黄和罗丹明B采用正离子模式,酸性橙采用负离子模式,建立正负离子切换的多反应监测(MRM)的检测方法。结果碱性橙Ⅱ、碱性嫩黄O的检出限为1.0g/kg,酸性橙Ⅱ和罗丹明B的检出限为0.5g/kg,方法回收率为84.295.1%,相对标准偏差(RSD)小于4.5%。结论建立的液质联用方法具有快速、灵敏、准确等优点,可用于豆制品中上述4种非法添加的红黄色系工业染料的同时测定及确证。
OBJECTIVE To establish a pretreatment method for the extraction of soybeans by the WAX solid phase extraction column with the prohibition of adding pigmented alkaline orange II, basic tender yellow O, acidic orange Ⅱ and rhodamine B respectively. Methods The electrospray ionization source (ESI), basic orange, basic yellow and rhodamine B were used in the positive ion mode and the acidic orange was used in the negative ion mode to establish the multi-reaction monitoring (MRM) detection method. Results The detection limit of alkaline orange II and basic yellow O was 1.0g / kg, the detection limit of acidic orange Ⅱ and rhodamine B was 0.5g / kg, the recovery was 84.295.1%. The relative standard deviation RSD) is less than 4.5%. Conclusion The established liquid chromatography-mass spectrometry method is rapid, sensitive and accurate. It can be used for the simultaneous determination and confirmation of the above three kinds of illegally-added industrial dyes in soy products.