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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 To establish a liquid chromatography fluorescence method for the determination of ethoxyquin residues in many kinds of food. Methods The samples were extracted with n-hexane under alkaline conditions and then detected by liquid-liquid extraction after pH adjustment. The chromatographic separation was carried out on an Agilent Eclipse XDB-C18 column (150 mm × 4.6 mm, 5 μm). A linear gradient of methanol-water was used as the mobile phase. The flow rate was 1.0 ml / min and the column temperature was 30 ℃. Excitation wavelength 365 nm, emission wavelength 425 nm. Results The calibration curve was linear with the concentration of ethoxyquin in the range of 0.05-10 mg / L (r = 0.999 2). The detection limit (S / N = 3) was 7.5 μg / ) Was 25μg / kg. The average recoveries were 80.5% ~ 95.9% and RSD were 3.1% ~ 11.5% (n = 8). Conclusion This method is practical and easy to operate and is suitable for the determination of ethoxyquin residues in many kinds of food.