超高效液相色谱电喷雾串联四极杆质谱法检测豆制品中12种禁用工业染料

Determination of 12 Banned Dyes in Soy Products by Ultra Performance Liquid Chromatography with Electospray Ionization Tandem Mass Spectrometry

建立了超高效液相色谱-电喷雾串联四极杆质谱（UPLC-MS/MS）同时检测豆制品中12种橙黄色工业染料（碱性橙2、碱性橙21、碱性橙22、苏丹黄、苏丹橙G、二乙基黄、碱性嫩黄O、溶剂黄124、酸性橙Ⅱ、酸性间胺黄、酸性黄11和茜素黄R）的分析方法。样品经酸化乙腈提取;提取液于-20℃冷冻2 h后离心,可有效去除豆制品中的脂质类干扰物;梯度洗脱条件下经ACQUITY UPLCBEH C18柱（1.7μm,2.1 mm×100 mm）分离后采用多离子反应监测模式（MRM）检测,4种工业染料（酸性橙Ⅱ、酸性间胺黄、酸性黄11和茜素黄R）使用负离子模式,以乙腈-0.1%氨水为流动相,其余8种采用正离子模式检测,流动相为乙腈-0.1%甲酸水。结果表明：豆制品中12种工业染料的定量下限（LOQ）为0.2-10.0μg/kg,3个加标水平的回收率为76.2%-122.0%,相对标准偏差为1.1%-7.4%,各项指标满足食品中痕量污染物检测的需要。该方法操作简便、灵敏度高,实现了12种禁用橙黄色染料的同时提取和净化,适合于豆制品中非法添加工业染料的筛查、确证。

An analytical method was developed for the simultaneous determination of 12 banned dyes（basic orange 2,basic orange 21,basic orange 22,dimethyl yellow,ethyl yellow,sudan orange G,auramine O,solvent yellow 124,orange Ⅱ sodium salt,metanil yellow,acid yellow 11 and allzarin yellow R） in soy products by ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS / MS）.Soy products samples were extracted using acetonitrile acidified with acetic acid.After frozen for 2 h under-20 ℃,the extracts were centrifuged to reduce lipids and other related interference.The target compounds were separated on an ACQUITY UPLC BEH C18 column by means of a binary mobile phase gradient with water containing 0.1% ammonium hydroxide formic acid and acetonitrile for 4 dyes（orange Ⅱ sodium salt,metanil yellow,acid yellow 11 and allzarin yellow R） and 0.1% formic acid and acetonitrile for the other eight compounds.Mass spectrometric acquisition was carried out by means of multiple reaction monitoing（MRM） under negative ionization mode for 4 dyes and positive mode for the rest of target compounds,respectively.As a result,quantitation limits of 12 dyes in soy products samples were in the range of 0.2-10.0 μg / kg.Mean recoveries at three spiked levels ranged from 76.2% to 122.0%,and the relative standard deviations（RSDs） were between 1.1% and 7.4%,which complied with the regulations for the determination of trace contaminants residues in food matrix.Simultaneous extraction and purification of 12 dyes in soy products matrix was achieved upon the established method which could be applied in theroutine detection of illegally additive dyes in soy products due to its simplicity and high sensitivity.