超高效液相色谱-串联四极杆质谱联用分析鸭蛋黄中的苏丹红Ⅰ～Ⅳ

Determination of Sudan Red Ⅰ-Ⅳ in Duck Egg Yolk Using Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了鸭蛋黄中苏丹红Ⅰ～Ⅳ号的超高效液相色谱-串联四极杆质谱联用(UPLC-MS/MS)的分析方法。采用乙腈提取样品中的苏丹红,加水反沉淀除去蛋白质和脂肪等杂质,冷冻后高速离心,取上层清液供UPLC-MS/MS分析。经Waters Acquity BHE C18超高效液相色谱柱分离,串联四极杆质谱多反应监测模式检测,4种物质的检出限均为0.05μg/L,实际样品中4种物质的检出限为10μg/kg。采用标准添加法测定苏丹红的回收率,100.0,200.0,300.0μg/kg3个不同添加水平的回收率为50.2%～101.3%。实验结果表明该方法灵敏度高,检出限低,确证能力强,分析时间短,可满足高通量食品样品中苏丹红的日常检测。

A method of the simultaneous analysis of Sudan Red Ⅰ - Ⅳ in duck egg yolk was developed with an ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. Acetonitrile was used to extract the residues from duck egg yolk, and water was added into the extract to precipitate impurities such as protein and fat. The supernatant was detected by the UPLC-MS/MS after refrigeration and centrifugation. The sample was separated on a Waters Acquity BHE C18 column, and detected by MS/MS with the multiple reaction monitoring （MRM） mode. The limits of detection （LOD） were 0. 05 μg/L in the standard solution, and 10 μg/kg of the four substances in the sample spiked with Sudan Red Ⅰ - Ⅳ. The average recoveries were between 50.2% - 101.3% at three spiking levels of 100.0, 200.0, 300.0 μg/kg. The experiment results show that this method is of high sensitivity, low LOD, better determination capacity and shorter analysis time. The method could meet the high-throughout detection of Sudan Red in food samples.