摘要
目的建立调味品中苏丹橙、苏丹黄、苏丹Ⅰ~Ⅳ、溶剂蓝35、对位红、苏丹黑B、苏丹红7B、苏丹红G、苏丹棕等工业染料的固相萃取-超高效液相色谱串接四级杆质谱(SPE-UPLC-MS/MS)测定方法。方法以含10%乙醇的丙酮溶液作为提取溶剂,利用MAX强阴离子交换固相萃取柱(60mg,3ml)对样品进行净化,UPLC-MS/MS测定试样中12种工业染料的含量。结果方法的线性范围:对位红10.0~800.0ng/ml,其他11种染料5.0~400.0ng/ml。12种工业染料的定性检出限为0.3~10.4μg/kg。定量检出限为0.8~31.2μg/kg。高、中、低3个浓度水平的加标回收率77.1%~141.9%,相对标准偏差5.5%~26.4%。结论本方法灵敏、准确,可用于调味品中苏丹橙、苏丹黄、苏丹Ⅰ~Ⅳ、溶剂蓝35、对位红、苏丹黑B、苏丹红7B、苏丹红G、苏丹棕等12种非法添加的工业染料的同时测定及确证。
Objective To established a method for simultaneous determination of Sudan Orange,Sudan Yellow,Sudan Ⅰ-Ⅳ,Solvent Blue 35,Para Red,Sudan Black B,Sudan Red 7B,Sudan Red G and Sudan Brown in condiment by solid-phase extraction and ultra performance liquid chromatography electrospray ionization-tandem mass spectrometry (SPEUPLC-MS /MS) method.Method The samples were extracted by acetone containing 10% ethanol and cleaned-up by OASIS MAX solid phase extraction column (60 mg,3 ml).The dyes were determined by UPLC-MS /MS.Results The linear range was 10.0-800.0 ng /ml for Para Red and 5.0-400.0 ng /ml for the other 11 compounds,the correlation coefficients were0.99.The qualitative detection limits of the method were in the range of 0.3-10.4 μg /kg and the quantitative detection limits of the method were in the range of 0.8-31.2 μg /kg.The average recoveries of adding standard at three levels were 77.1%-141.9% and the relative standard deviation (RSD) of the method was 5.5%-26.4%.Conclusion The method is sensitive,accurate and could be used for detecting 12 kinds of industrial dyes simultaneously in condiments.
出处
《中国食品卫生杂志》
北大核心
2010年第4期305-312,共8页
Chinese Journal of Food Hygiene
基金
北京市卫生局
北京市中医管理局青年科学研究资助项目(QN2007-16)