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建立了固相萃取净化和凝胶色谱净化两种前处理方法,应用高效液相色谱串联质谱法同时测定了食品中苏丹红Ⅰ,Ⅱ,Ⅲ和Ⅳ,对位红、罗丹明B 6种禁用染料。根据不同的净化技术,分别选用甲醇和乙酸乙酯-环己烷(1:1,V:V)作为提取溶剂,利用C8色谱柱(1.8μm,3.0×100 mm)分离,电喷雾串联四极杆质谱ESI源,在多反应监测模式下对6种禁用染料进行检测。用相萃取净化方法苏丹红Ⅰ,Ⅱ,Ⅲ,Ⅳ和对位红的检出限为0.005 mg/kg,罗丹明B的检出限为0.002 mg/kg;疑胶色谱净化方法苏丹红Ⅰ,Ⅱ,Ⅲ,Ⅳ和对位红的检出限为0.010 mg/kg,罗丹明B的检出限为0.005 mg/kg。通过比较两种净化方法在检测复杂基质中的实际应用,固相萃取净化法在去除大分子物质、天然色素方面的效果好于凝胶色谱净化法。
Two pretreatment methods, solid phase extraction and gel filtration, were established. The simultaneous determination of Sudan Ⅰ, Ⅱ, Ⅲ and Ⅳ in food and banned red and rhodamine B by high performance liquid chromatography tandem mass spectrometry dye. According to different purification technologies, methanol and ethyl acetate-cyclohexane (1: 1, V: V) were selected as the extraction solvent and separated by C8 column (1.8μm, 3.0 × 100mm) Rod mass ESI source, 6 prohibited dyes were tested in a multi-reaction monitoring mode. The detection limit of Sudan Ⅰ, Ⅱ, Ⅲ, Ⅳand Para red was 0.005 mg / kg by phase extraction and the detection limit of rhodamine B was 0.002 mg / kg. The purifying method of polyglutamic acid was Sudan Ⅰ, The detection limit of Ⅱ, Ⅲ, Ⅳ and para red was 0.010 mg / kg, and the detection limit of rhodamine B was 0.005 mg / kg. By comparing the practical application of the two purification methods in the detection of complex matrices, the SPE purification method is better than the gel chromatography purification method in removing macromolecules and natural pigments.