[关键词]
[摘要]
本研究成功建立了QuEChERS净化液相色谱-串联质谱内标法同时测定调味品中11种工业染料(碱性嫩黄O、碱性黄、碱性橙21、碱性橙22、碱性橙2、罗丹明B、罗丹明6G、苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅲ和苏丹红Ⅳ)的分析方法。样品经乙腈提取,采用C18和PSA吸附剂净化后进行液相色谱-串联质谱分析,多反应监测(MRM)模式检测,内标法定量。结果表明,在0.5~100 μg/L范围内,方法呈现良好的线性关系(r>0.9976),检出限在0.01~0.4 μg/kg之间。当实际样品中添加水平为5~200 μg/kg时,方法平均回收率为70.7%~105.0%,相对标准偏差(RSD)为0.1%~9.3%。应用本方法对50个批次的调味品进行测定,发现其中4个批次样品检出不同浓度的罗丹明B。该方法操作简便,快速准确,可以用于调味品中11种非法添加工业染料残留的测定。
[Key word]
[Abstract]
A fast and sensitive method for the simultaneous determination of 11 industrial dyes (auramine O, basic yellow, basic orange 21, basic orange 22, basic orange 2, rhodamine B, rhodamine 6G, Sudan red I~IV) in condiments was successfully established with QuEChERS (quick, easy, cheap, effective, rugged, and safe)-based purification and liquid chromatography–tandem mass spectrometry (internal standard method). The industrial dyes were extracted with acetonitrile and further purified with QuEChERS method using C18 and primary-secondary amine (PSA) to reduce the matrix interference. Subsequently, the sample was analyzed by liquid chromatography–tandem mass spectrometry under multiple reaction monitoring (MRM) mode, and the internal standard method was used for quantitative analysis. The results showed that the method had a good linearity in the range of 0.5~100 μg/L (R2=0.9976), and the limits of detection (LODs) were in the range of 0.01~0.4 μg/kg. The average recoveries of industrial dyes from spiked condiments ranged from 70.7 to 105.0%, and the relative standard deviations were between 0.1 and 9.3%. This method was applied to analyze 50 batches of condiment samples, and different concentrations of rhodamine B were found in four of them. The results indicated that the developed method was fast and accurate, and could be applied for the detection of residues of 11 industrial dyes illegally added in the condiments.
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[基金项目]
国家自然科学青年科学基金项目(21605028);广州市科技计划项目(201704020024);广州市科技计划项目(2014J4100196);广东省省级科技计划项目(2016A020210102);广东省食品质量安全重点实验室(华南农业大学)开放课题(2015)