液相色谱荧光法测定食品中乙氧基喹残留量
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郑国灿 男 工程师 研究方向为食品安全监测技术 E-mail:ciqzgc2007@126.com

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国家质检总局科研制标项目(2009B523)


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

    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(150mm×4.6mm,5μm)色谱分离,甲醇-水为流动相进行线性梯度洗脱,流速为1.0ml/min,柱温30℃,进样量20μl;荧光检测器激发波长365nm,发射波长425nm。结果 乙氧基喹在0.05~10mg/L范围内线性关系良好(r=0.9992),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。

    Abstract:

    A method for the determination of ethoxyquin residue in food by liquid chromatography with fluorescence detector was developed.MethodsThe 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(150mm×4.6mm, 5μm) with a gradient elution using methanol-water as mobile phase at a flow rate of 1.0ml/min, the column temperature was 30℃, and the injection volume was 20μl. The ethoxyquin was detected under FD at λexem=365nm/425nm.Results The linear range of ethoxyquin was 0.05-10mg/L, and the correlation coefficient was 0.9992. The limit of detection was 7.5μg/kg (S/N=3) and the limit of quantification was 25μg/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.

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郑国灿,朱美文,王晶,尹楠戈,彭光宇,陈江,李贤良.液相色谱荧光法测定食品中乙氧基喹残留量[J].中国食品卫生杂志,2013,25(5):424-427.

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  • 收稿日期:2013-05-21
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  • 在线发布日期: 2013-10-25
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