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目的建立一种凝胶渗透色谱-高效液相色谱法(gel permeation chromatography-high performance liquid chromatography,GPC-HPLC)同时测定糟蛋中4种苏丹红(苏丹红Ⅰ、Ⅱ、Ⅲ和Ⅳ)的方法。方法糟蛋样品经环己烷-乙酸乙酯提取,经Bio-Beads S-X3凝胶柱净化;采用Agilent Zorbax SB C_(18)色谱柱对糟蛋中4种苏丹红进行分离,以97%乙腈水溶液为流动相,流速为1.0 m L/min,用配有紫外检测器的液相色谱仪检测,检测波长为478 nm和520 nm。结果 4种苏丹红样品在0.1~25.0 mg/L浓度范围内线性良好(r~2>0.999),该方法的检测限为6.3~11.9μg/kg,加标回收率为86.0%~101.2%,相对标准偏差(RSD)在1.68%~4.58%之间。结论本方法操作简便、准确可靠,可应用于糟蛋中苏丹红的检测。
OBJECTIVE To establish a method for simultaneous determination of four Sudan Reds (Sudan I, II, III and IV) in a dregs by gel permeation chromatography-high performance liquid chromatography (GPC-HPLC) . Methods The samples of bad eggs were extracted with cyclohexane-ethyl acetate and purified by Bio-Beads S-X3 gel column. The four Sudan reds were separated by Agilent Zorbax SB C_ (18) Acetonitrile as the mobile phase at a flow rate of 1.0 m L / min using a liquid chromatograph with a UV detector at 478 nm and 520 nm. Results The four Sudan samples showed a good linearity (r ~ 2> 0.999) within the range of 0.1 ~ 25.0 mg / L. The detection limits were 6.3 ~ 11.9 μg / kg and the recoveries were 86.0% -101.2% The relative standard deviations (RSDs) ranged from 1.68% to 4.58%. Conclusion The method is simple, accurate and reliable and can be applied to detect Sudan in bad eggs.