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目的建立食品中6种工业染料的QuEChER前处理高效液相色谱-串联质谱同时测定方法。方法均匀样品用水分散溶解后,加乙腈提取,经改进的QuEChERS方法净化,0.22μm微孔滤膜过滤,用0.1%甲酸-5mmol/L乙酸铵溶液和乙腈为流动相梯度洗脱,C_(18)柱分离,分别在电喷雾正、负离子模式下以多反应监测方式检测,外标法定量。结果结果表明,6种工业染料在0.5~40μg/L浓度范围内与其呈良好的线性关系(r>0.999),检出限为1.0~2.0μg/kg,在添加水平为1.0、5.0、20μg/kg时,平均回收率为76.1%~114.8%,相对标准偏差(RSD)为2.0%~9.7%(n=6)。结论该方法分析速度快,灵敏可靠,重复性好,适用于调味品、豆制品、卤肉制品、红糖等食品中6种工业染料的测定。
Objective To establish a method for the simultaneous determination of six kinds of industrial dyes in food by QuEChER pretreatment with high performance liquid chromatography-tandem mass spectrometry. Methods The sample was homogenized with water, dissolved in water, extracted with acetonitrile, purified by a modified QuEChERS method and filtered through a 0.22 μm microporous membrane filter. The mobile phase was eluted with 0.1% formic acid in 5 mmol / L ammonium acetate and acetonitrile as mobile phase. ) Column separation, respectively, in electrospray positive and negative ion mode to multiple reaction monitoring, external standard method. The results showed that the six industrial dyes had a good linear relationship (r> 0.999) with the concentration range of 0.5-40 μg / L, the detection limit was 1.0-2.0 μg / kg, and at the addition level of 1.0, 5.0 and 20 μg / kg, the average recoveries ranged from 76.1% to 114.8% and the relative standard deviations (RSDs) ranged from 2.0% to 9.7% (n = 6). Conclusion The method is rapid, sensitive, reliable and reproducible. It is suitable for the determination of six industrial dyes in condiments, soy products, braised meat products and brown sugar.