LC-MSMS测定染色黄鱼中碱性橙的残留.pdfVIP

LC-MS/MS 测定染色黄鱼中碱性橙的残留 寿林飞* 黄百芬 铁晓威 任一平 浙江省疾病预防控制中心 杭州 310009 摘要：本实验建立了新鲜黄鱼中的碱性橙残留的液相色谱-电喷雾串联四级质谱的定性、定量分 析方法。样品经去头去尾去骨，以及粉碎、匀浆后经 1moL/L 盐酸溶液振荡提取，离心后过 Waters Oasis HLB 柱固相萃取净化处理。经液相色谱分离，质谱多离子反应监测（multiple-reaction monitoring, MRM）定量。最低检测限(LOD)为 0.072ng。而最低定量（LOQ）为 0.24ng/mL。加标 回收率为 96.7%，在 0.625-40ng/mL 的浓度范围内线性关系良好，r2=0.9999；6 次重复取样测定 RSD 为 0.32% 。 关键词：液相色谱－电喷雾串联四极质谱; 碱性橙; 固相萃取；染色黄鱼 Determination of Basic Orange Residue in Yellow-fin Tuna By Liquid Chromatography Tandem Mass Spectrometry SHOU Lin Fei HUANG Bai Fen TIE Xiao Wei REN Yi Ping Zhejiang Provincial Center for Disease Prevention and Control ，Hangzhou 310009 Abstract: This paper describes a newly developed HPLC-MS/MS method for determination of basic orange in yellow-fin tuna. Multiple reaction monitoring (MRM) was employed for quantitative determination. Samples were prepared by homogenizing the tissue, extracting with 1 mol/L hydrochloric acid. For clean-up and concentration, solid phase extraction (SPE) with OASIS HLB cartridges were used. The detection limit of this method was 0.072 ng/ml，and limit of quantification (LOQ) was 0.24 ng/ml. The mean recovery was 96.7%. The linear range was from 0.625 to 40ng/mL with correlation coefficients of 0.9999. The relative standard deviation (RSD) was 0.32% (n=6). Key words: LC-MS/MS, Basic Orange ，Yellow-fin Tuna 碱性橙是一种偶氮类碱性工业染料，用于腈纶、蚕丝、羊毛、二醋纤、单宁媒纤维的染色，染 腈纶牢度尚可，也可以用于皮革、麻的染色和竹、木、纸张、蚊香的着色及制造色淀、溶剂染料、 阳离子染料[1]。分子式:C H N .HCL 相对分子量:248.72，在溶液中成为游离态，其结构见图 1。该 12 12 4 物质属偶氮类染料，已被认定是一种可以使人致癌的物质，不得用于与人体长期直接接触的纺织和 服装产品中，而被用作食品染色剂更是严加禁止，根据《中华人民共和国食品添加剂使用卫生标准》 (GB2760)及《中华人民共和国食品卫生法》的相关现定，碱性橙为禁止用作食品添加剂的化学制品 [2] 。 图 1 碱性橙的分子结构式 由于碱性橙比食用色素更易于在鱼类表皮着色；且不易褪色，经染色后的杂鱼和养殖黄鱼的表 面颜色与野生黄鱼完全一样。因此不