豆制品中15种工业染料的超快速液相色谱串联四级杆质谱快速筛查法

Rapid screening for 15 kinds of industrial dye in soybean products by ultra-performance liquid chromatography tandem mass spectrometry

目的建立豆制品中非法添加的15种工业染料超快速液相色谱串联四级杆质谱的快速监测方法。方法样品用乙腈作为提取液，过0．22μm的滤膜直接经C18柱梯度洗脱，正离子模式流动相为甲醇和0．1％的甲酸水溶液，负离子模式流动相为甲醇和纯水。采用多反应监测（MRM）模式进行检测，其中13种化合物设定为正离子模式，2种化合物为负离子模式。采用基质匹配的外标方法进行定量。结果豆干中15种工业染料的检出限为0．2—10μg／kg、定量限为0．6—30μg/kg、回收率为60．1％～113．5％、相对标准偏差为1．1％～14．9％。结论该方法检测时间短，灵敏度高，操作简便，同时用正负离子检测15种不同的工业染料在豆制品中的添加情况，可以根据不同要求添加新的工业染料，同时也可以根据要求变化基质检测其他食品。

[ Objective] To established a rapid method of screening for 15 kinds of industrial dye in soybean products by ultra-per- formance liquid chromatography tandem mass spectrometry. [ Methods ] The samples were extracted by acetonitrile. In the gradient elution conditions, the samples were gone through a 0.22 μm filter membrane, and separated by C18 column. The mobile phase was methanol with 0.1% formic acid solution in the ESI（ ＋ ） mode and methanol with water in the ESI（-） mode. 15 kinds of in- dustrial dyes were detected by muhiple reaction monitoring （MRM） mode. Among them, 13 kinds of industrial dyes were detected in ESI（ ＋ ） mode and 2 kinds were detected in the ESI（-） mode. The matrix matching and external standard method was applied in the quantitative analysis. [ Results] The resuhs of the 15 kinds of industrial dyes in bean products were as follows： the detection limit was 0.2-10 μg/kg, the limit of quantification was 0.6-30 μg/kg, the coefficient of recovery was 60. 1% -113.5%, and the relative standard deviation was 1.1% -14.9%. [ Conclusion ] This method has the short detection time, the high sensitivity, and the simple operation steps. It can determine the residues of 15 kinds of industrial dyes in bean products in the different mode at the same time. Meanwhile, this method can continue to increase the variety of industrial dyes, and detect other food by changing matrix according to requirements.