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[摘要]
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。10 mL乙腈-二氯甲烷(3:2,V/V)混合溶液作为提取液,依次用10 mL正己烷、4 mL乙酸乙酯-正己烷(1:1,V/V)混合溶液作为淋洗液,12 mL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 BEH C18色谱柱(2.1×100 mm,1.7 μm),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~ 500 μg/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、4.0 μg/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。
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[Abstract]
Using a basic alumina column, which has stronger reaction with sudan dye, as a solid phase extraction (SPE) column, an ultra-high performance liquid chromatography-tandem quadrupole mass spectrometry (UPLC-MS) method was developed for the determination of four sudan dyes in chili products. The extraction solvent, washing liquid for the SPE column, eluent solvent, and liquid chromatography conditions were optimized separately. The sudans were extracted by using 10 mL mixed acetonitrile and dichloromethane solution (3:2, V/V) was used to extract the Ten milliliters of n-hexane and 4 mL mixed ethyl acetate and n-hexane (1:1, V/V) were used as washing liquids. Twelve milliliters of a mixed 5% acidified methanol and ethyl acetate solution (1:1, V/V) was used for elution. An ACQUITY BEH C18 chromatography column (2.1 × 100 mm, 1.7 μm) was used with mobile phases composed of 0.3% formic acid acetonitrile solution and 0.3 % formic acid water solution. The substrate spiked standard curves of the four sudan dyes had good linear correlations in the range 10~500 μg/L, with all correlation coefficients above 0.995. The limits of detection (LOD) of the four sudan dyes were 5.0, 5.0, 4.0, and 4.0 μg/kg. The recovery experiment, performed by adding samples, was carried out with blank samples at concentrations between 10-150 μg/kg. The average recovery ratio was 71.4%~104.2%, and the relative standard deviation (RSD, n = 6) was 4.6%~8.9%. Three hundred and eighty samples were examined using this method, and 36 samples were positive for sudans, and the component was primarily sudan IV.
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