固相萃取结合超高效液相色谱-串联质谱法同时检测食品中的6种工业染料  

Simultaneous Determination of 6 Industrial Dyes in Foods by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：曹鹏[1,2] 乔旭光[1] 娄喜山 耿金培 付建 张禧庆 

机构地区：[1]山东农业大学食品科学与工程学院,泰安271018 [2]烟台出入境检验检疫局,烟台264000 [3]烟台杰科检测服务有限公司,莱阳265231

出　　处：《分析化学》2011年第11期1670-1675,共6页Chinese Journal of Analytical Chemistry

基　　金：山东检验检疫局科技攻关项目(No.SK200936)资助

摘　　要：建立了超高效液相色谱一串联质谱（UPLC-MS／MS）同时检测食品中6种工业染料含量的方法。样品用含50％甲醇和1％甲酸的50mmol／L乙酸铵溶液进行提取、WAX弱阴离子交换固相萃取柱进行净化后，采用多反应监测（MRM）模式进行检测，基质曲线外标法定量。其中酸性橙Ⅱ采用负离子模式检测，其余5种染料采用正离子模式检测。碱性橙Ⅱ、罗丹明B、碱性嫩黄O、罗丹明6G、碱性桃红T的定量限为1．6μg／kg，酸性橙Ⅱ为6．0μg／kg；碱性橙Ⅱ、罗丹明B、碱性嫩黄O、罗丹明6G、碱性桃红T的线性范围为1．0～100．0μg／L；酸性橙Ⅱ的线性范围为5．0～100pg／L，线性相关系数均大于0．999。6种染料的回收率为70．3％～109．2％；相对标准偏差（RSD）为2．6％～14．1％。本方法灵敏度高，操作简单高效，适合于食品中6种非法添加工业染料的定量及确证分析。An ultra high performance liquid chromatography-tandem mass spectrometric method was established for the simultaneous determination of the residues of six industrial dyes in foods. The samples were extracted with 50 mmol/L ammonium acetate solution containing 50% methanol and 1% formic acid, cleaned up by WAX solid phase extraction column, and then analyzed in multiple reaction monitoring （MRM） mode. Sample matrix-matched calibration was used to determine the residue contents by external standard. Orange Ⅱ was detected with negative ion model, and the other five dyes were detected with positive ion model. Limit of quantitation （LOQ） of Chrysoidine Ⅱ, Rhodamine B , Auramine O , Rhodamine 6G and Safranine T was 1.6 μg/kg,and LOQ of orangeⅡ was 6.0 μg/kg. The linear range of chrysoidine Ⅱ , rhodamine B, auramine O, rhodamine 6G and safranine T was 1.0-100.0μg/L and that of orange Ⅱ was 5.0-100.0μg/L, the linear correlation coefficients were all more than 0. 999. The recoveries of 6 dyes ranged from 70.3% to 109.2% with relative standard deviations （RSD） of 2.6%-14.1%. This method was simple, effective and sensitive, and was suitable for the determination and confirmation of six industrial dyes added in the foods illegally.

关 键 词：超高效液相色谱-串联质谱法 碱性橙Ⅱ 罗丹明B 碱性嫩黄O 碱性桃红T 罗丹明6G 酸性橙Ⅱ 食品 

分 类 号：TS207.3[轻工技术与工程—食品科学] O657.63[轻工技术与工程—食品科学与工程]