凝胶柱净化-高效液相色谱检测食品中的苏丹红

Simultaneous Determination of Sudan Red Dyes in Foods by High Performance Liquid Chromatography with a Clean-Up Procedure by Gel Column

建立了凝胶柱净化-高效液相色谱同时检测食品中苏丹红Ⅰ,Ⅱ,Ⅲ和Ⅳ的方法.样品用乙醇提取,提取液经Bio-Beads SX3凝胶柱(200 mm×10 mm i.d.)净化,用环己烷-乙酸乙酯(体积比为1:1)洗脱.采用Symmetry Shield RP18柱(250 mm×4.6 mm i.d., 5 μm)分离,以100%甲醇为流动相,流速1.5 mL/min;用二极管阵列检测器检测,检测波长478 nm.上述4种苏丹红组分在其质量浓度为0.1～10.0 mg/L时有良好的线性关系(r>0.999),方法的检测限为7～14 μg/kg;平均加标回收率为80.7% ～96.3% (添加水平为0.25,2.5 mg/kg),相对标准偏差为2.4% ～5.9% .方法灵敏可靠,能满足食品中苏丹红检测的需要.

A method was developed for the simultaneous determination of Sudan Red Ⅰ , Ⅱ, Ⅲ and IV in foods by high performance liquid chromatography （HPLC） with a clean-up procedure by gel column, Sample was extracted from foods with ethanol. The extract was cleaned up with a Bio-Beads SX3 gel column （200 mm× 10 mm i. d. ） and eluted with cyclohexane-ethyl acetate （1： 1, v/v）. The analysis was performed on a Symmetry Shield RP18 column （250 mm × 4, 6 mm i. d, , 5 μm） with 100% methanol as the mobile phase at a flow rate of 1.5 mL/min, detection at 478 nm and confirmation by diode-array spectra. All of the four compounds demonstrated good linear relationship （r 〉 0. 999） in the range of 0. 1 - 10, 0 mg/L. The limits of detection （LOD） were from 7 to 14 μg/kg, The average recoveries for all four dyes （spiked at the levels of 0.25 and 2, 5 mg/kg） in chili sauce and sausage ranged from 80.7% to 96.3%, and the relative standard deviations were from 2.4% to 5.9%. The method is sensitive, reliable and can be applied for the analysis of four Sudan Red dyes in foods.