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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 establish a rapid monitoring method for ultra-fast liquid chromatography tandem quadrupole mass spectrometry of 15 industrial dyes illegally added to soy products. Methods The sample was eluted with acetonitrile as the extract, and the filtrate was filtered through a C18 column with a 0.22 μm membrane. The mobile phase of positive ion was methanol and 0.1% formic acid. The mobile phase was methanol and pure water. Multiple reaction monitoring (MRM) patterns were used for the detection, of which 13 compounds were set as the positive ion mode and the two compounds were the negative ion mode. Matrix-matched external standard method for quantification. Results The detection limits of 15 industrial dyes were 0.2 ~ 10μg / kg, the limits of quantification was 0.6 ~ 30μg / kg, the recoveries were 60.1% ~ 113.5% and the relative standard deviations were 1.1% ~ 14.9%. Conclusion The method has the advantages of short detection time, high sensitivity and easy operation. At the same time, the addition of 15 different industrial dyes to soy products by using positive and negative ions can be added according to different requirements and can be changed according to requirements. Other food.