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目的:建立同时测定食品中非法添加的罗丹明B和苏丹红工业染料的液相色谱-串联离子阱质谱法。方法:样品经正己烷提取、中性氧化铝固相萃取柱净化后,以甲醇(A)和1%甲酸(B)为流动相经BioBasic-18 PIONEER柱(150 mm×2.1 mm,5μm)梯度洗脱分离,串联离子阱质谱在电喷雾电离正离子(ESI+)-全扫描(full)-二级质谱(MS/MS)模式下测定罗丹明B和苏丹红含量。结果:方法的线性范围:罗丹明B0 ng/ml～20 ng/ml,苏丹红0 ng/ml～100 ng/ml,r≥0.992。方法的定性检出限为:罗丹明B与苏丹红I、II、III、IV分别为0.1μg/kg、0.5μg/kg、5.0μg/kg、2.0μg/kg、2.0μg/kg。罗丹明B与苏丹红在3种基质高、低两个浓度水平的加标回收率85.2%～109.5%,精密度<20%。结论:本方法灵敏、准确,可用于食品中罗丹明B和苏丹红等非法添加的工业染料的同时测定及确证。
Objective: To establish a liquid chromatography - tandem ion trap mass spectrometry method for the simultaneous determination of illegally added rhodamine B and Sudan dyes in food. Methods: After the sample was extracted with n-hexane and purified by a neutral alumina solid-phase extraction column, the sample was separated on a BioBasic-18 PIONEER column (150 mm × 2.1 mm, 5 μm) with methanol (A) and 1% formic acid Elution separation, tandem ion trap mass spectrometry Rhodamine B and Sudan content were determined by electrospray ionization positive ion (ESI +) - full-scan mass spectrometry (MS / MS) mode. Results: The linear range of the method was: rhodamine B 0 ng / ml ~ 20 ng / ml, Sudan red 0 ng / ml ~ 100 ng / ml, r ≥ 0.992. The qualitative detection limit of the method was: 0.1μg / kg, 0.5μg / kg, 5.0μg / kg, 2.0μg / kg and 2.0μg / kg respectively for rhodamine B and Sudan red I, II, III and IV. Rhodamine B and Sudan red in three kinds of matrix high and low levels of the two spiked recoveries 85.2% ~ 109.5%, precision <20%. Conclusion: The method is sensitive and accurate and can be used for the simultaneous determination and confirmation of industrial dyes illegally added in foods such as rhodamine B and Sudan red.