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本文采用与苏丹红染料作用更强的碱性氧化铝柱为固相萃取小柱,建立了超高效液相色谱-质谱法测定辣椒制品中4种苏丹红的测定方法。分别对提取溶剂、固相萃取小柱淋洗液、洗脱液及液相色谱条件进行了优化。10mL乙腈-二氯甲烷(3:2,V/V)混合溶液作为提取液,依次用10mL正己烷、4mL乙酸乙酯-正己烷(1:1,V/V)混合溶液作为淋洗液,12mL的5%酸化甲醇-乙酸乙酯(1:1,V/V)混合溶液作为洗脱液。采用ACQUITY BEHC18色谱柱(2.1×100mm,1.7μm),以0.3%甲酸乙腈溶液,0.3%甲酸水溶液为流动相,等度洗脱。4种苏丹红基质添加标准曲线在10~500μg/L的浓度范围内有良好的线性关系,线性相关系数均大于0.995。苏丹Ⅰ~Ⅳ的检出限分别为5.0、5.0、4.0、4.0μg/kg。在10~150μg/kg浓度范围做空白样品添加实验,平均回收率在71.4~104.2%之间,相对标准偏差(RSD,n=6)在4.6~8.9%之间。应用本方法测试380份样品,其中阳性样品36份,阳性样品检出组分主要为苏丹Ⅳ。
In this paper, a solid-phase extraction column with basic alumina column which is stronger than Sudan dyes was used to establish a method for the determination of four Sudan reds in pepper products by ultra performance liquid chromatography-mass spectrometry. Solvent extraction, solid-phase extraction cartridge eluent, eluent and liquid chromatography conditions were optimized. 10 mL of acetonitrile-dichloromethane (3: 2, V / V) as the extract, followed by 10 mL of n-hexane and 4 mL of ethyl acetate-n-hexane 12 mL of 5% acidified methanol-ethyl acetate (1: 1, v / v) mixed solution as eluent. An ACQUITY BEHC18 column (2.1 × 100 mm, 1.7 μm) was used and was eluted isocratically with 0.3% formic acid in acetonitrile and 0.3% formic acid in water. The standard curve of the four Sudan matrix additions had a good linearity in the concentration range of 10 ~ 500μg / L with the linear correlation coefficients greater than 0.995. The detection limits of Sudan Ⅰ ~ Ⅳ were 5.0, 5.0, 4.0 and 4.0 μg / kg, respectively. The blank samples were added in the range of 10 ~ 150μg / kg. The average recoveries ranged from 71.4% to 104.2%. The relative standard deviations (RSDs, n = 6) ranged from 4.6% to 8.9%. 380 samples were tested by this method, including 36 positive samples and the positive samples were mainly Sudan Ⅳ.