Determination of 11 Azo-dyes and Rhodamine B in Seasoning Oil by Gel Permeation Chromatography/Ultra Performance Liquid Chromatography with Electrospray Ionization Tandem Mass Spectrometry
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KeyWord:gel permeation chromatography(GPC)  ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)  azo-dyes  rhodamine B  seasoning oil  determination
赵珊,张晶,丁晓静,郭巧珍,邵兵 北京市疾病预防控制中心食物中毒诊断溯源技术北京市重点实验室
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      An analytical method was developed for the simultaneous determination of 11 banned azo=dyes (Sudan red Ⅰ,Sudan red Ⅱ,Sudan red Ⅲ,Sudan red Ⅳ,Sudan red 7B,Sudan red G,Sudan yellow,Sudan orange G,Sudan blue Ⅱ,toluidine red,para red) and rhodamine B in seasoning oil based on gel permeation chromatography followed by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The seasoning oil samples were extracted with cyclohexane-ethyl acetate(1∶1),and then purified by gel permeation chromatography to remove the high molecular weight of interferences(e.g.fat,oil and natural pigments).Twelve target compounds were separated on an ACQUITY UPLC- BEH C18 column with 0.1% formic acid and acetonitrile as mobile phase by gradient elution,and detected by MS/MS under positive mode with multiple reaction monitoring(MRM).Good linearities for 12 dyes were achieved over the range of 1-50 μg/L.The quantitation limits of 12 dyes in seasoning oil samples were in the range of 0.2-2.5 μg/kg.The mean recoveries at three spiked level(5,20,40 μg/L) ranged from 54% to 125%, with relative standard deviations(RSDs) of 2.5%-17.2%.The method was used to analyze 35 seasoning oil samples taken randomly from the local market,and rhodamine B was found in 2 of the samples.The established method could be applied in the simultaneous extraction and purification of 11 azo-dyes and rhodamine B in seasoning oil matrix,and is suitable for the routine detection of illegally additive dyes in seasoning oil due to its simplicity and high sensitivity.