液相色谱荧光法测定食品中乙氧基喹残留量  

Determination of ethoxyquin residue in food by liquid chromatography with fluorescence detector

作　　者：郑国灿[1] 朱美文[1] 王晶[1] 尹楠戈[2] 彭光宇[1] 陈江[1] 李贤良[1] 

机构地区：[1]重庆出入境检验检疫局,重庆400020 [2]重庆医科大学,重庆400016

出　　处：《中国食品卫生杂志》2013年第5期424-427,共4页Chinese Journal of Food Hygiene

基　　金：国家质检总局科研制标项目(2009B523)

摘　　要：目的建立检测多类食品中乙氧基喹残留量的液相色谱荧光法。方法样品在碱性条件下用正己烷提取,经调节酸碱度液液萃取净化后进行检测。采用Agilent Eclipse XDB-C18柱(150 mm×4.6 mm,5μm)色谱分离,甲醇-水为流动相进行线性梯度洗脱,流速为1.0 ml/min,柱温30℃,进样量20μl;荧光检测器激发波长365 nm,发射波长425 nm。结果乙氧基喹在0.05～10 mg/L范围内线性关系良好(r=0.999 2),方法的检出限(S/N=3)为7.5μg/kg,定量限(S/N=10)为25μg/kg;8类食品基质分别添加3个不同浓度水平,平均回收率为80.5%～95.9%,RSD为3.1%～11.5%(n=8)。结论本方法实用性强,可操作性好,适用于多类食品中乙氧基喹残留量的检测。Objective A method for the determination of ethoxyquin residue in food by liquid chromatography with fluorescence detector was developed.Methods The homogenized sample was extracted with n-hexane under alkaline conditions,then cleaned by liquid-liquid extraction(LLE) with n-hexane after adjusting the pH value.The targeted compound was determined by liquid chromatography-fluorescence detector.The chromatographic separation were achieved in Agilent Eclipse XDB-C18(150 mm×4.6 mm,5 μm) with a gradient elution using methanol-water as mobile phase at a flow rate of 1.0 ml/min,the column temperature was 30 ℃,and the injection volume was 20 μl.The ethoxyquin was detected under FD at λex/λem=365 nm/425 nm.Results The linear range of ethoxyquin was 0.05-10 mg/L,and the correlation coefficient was 0.999 2.The limit of detection was 7.5 μg/kg(S/N=3) and the limit of quantification was 25 μg/kg(S/N=10).In different food matrixes,the average recoveries of ethoxyquin under three spiked levels were 80.5%-95.9%,with RSDs(n=8) of 3.1%-11.5%.Conclusion This method was practical,maneuverable and suitable for the determination of ethoxyquin residue in various food.

关 键 词：乙氧基喹 液相色谱 荧光检测器 食品添加剂 抗氧化剂 食品安全 

分 类 号：R155.5[医药卫生—营养与食品卫生学] O657.72[医药卫生—公共卫生与预防医学]