凝胶净化/高效液相色谱-串联质谱法检测辣椒制品及肉制品中多种脂溶性着色剂

Determination of 11 fat-soluble colorants in chilli products and meat products by gel permeation chromatography/high performance liquid chromatography-tandem mass spectrometry

建立了凝胶渗透色谱净化／高效液相色谱-串联质谱测定辣椒制品和肉制品中苏丹橙G、甲基黄、对位红，柑桔红2号，苏丹红G，苏丹I，苏丹Ⅱ，苏丹Ⅲ，苏丹红7B，苏丹红B和苏丹Ⅳ的分析方法。样品经乙酸乙酯或乙腈-乙酸乙酯溶液提取后采用凝胶渗透色谱净化，通过ACQUITYHPLCBEHC18色谱柱以体积分数0．1％甲酸-体积分数0．1％甲酸甲醇溶液作流动相梯度洗脱分离，采用多反应监测模式进行检测。目标分析物使用同位素内标苏丹I—D5和苏丹Ⅳ-D6定量，11种待测物质量浓度在10～500ng／mL范围呈良好线性关系，相关系数大于0．99，方法的定量下限均达到5μg/kg。空白样品在5，10，20μg/kg3个加标水平下的平均回收率为80．7％-100．9％，相对标准偏差（n=10）均小于10％。

A method was developed for the determination of 11 fat-soluble colorants （Sudan Orange G, Dimethyl Yellow, Para Red, Citrus Red2, Citrus Red2, Sudan I , Sudan Ⅱ, Sudan Ⅲ, Sudan Red 7B, Sudan Red B, Sudan IV ） in chili products and meat products by gel permeation chromatography＇/ high performance liquid chromatography-tandem mass spectrometry. Sudan I -D5 and Sudan IV-D6 were the isotope internal standards. The sample was extracted by ethyl acetate or acetontrile-ethyl acetate and then purified by GPC. The targeted compounds were separated on an ACQUITY HPLC BEH Cls （ 100 mm× 2. 1 mm, 1.7 μm） column by using 0. 1% formic acid - 0. 1% formic acid / methanol solution as mobile phase, and detected by MS/MS in positive mode with multiple reaction monitoring （MRM）. Stable isotope-labeled analogues were used as the internalstandards for quantitation. The linear range of the target compounds ranged from 10 ng/mL to 500 ng/mL with correlation coefficients not less than 0. 99. The limits of detection （LLD） for the target compounds were 5 μg/ kg. The average recoveries at three spiked levels of 5, 10, 20 μg/kg were between 80. 7% and 100. 9%, with relative standard deviations （RSDs） less than 10%. The method could meet the requirements for routine analysis and actual detection.