高效液相色谱荧光检测法检测鸡蛋中阿莫西林残留

食品科学 ›› 2012, Vol. 33 ›› Issue (22): 264-268.

高效液相色谱荧光检测法检测鸡蛋中阿莫西林残留

谢恺舟1,2，陈学森 1,2，徐东1,2，郭辉生1,2 ，贾龙飞1,2 ，谢星3，黄玉萍1,2，张小杰1,2，孙瑛瑛1,2，戴国俊1,2，张跟喜1,2，王金玉1,2

1.扬州大学动物科学与技术学院 2.江苏省动物遗传繁育与分子设计重点实验室 3.南京农业大学动物医学院

收稿日期:2011-11-29 修回日期:2012-10-19 出版日期:2012-11-25 发布日期:2012-11-20
通讯作者: 谢恺舟 E-mail:kzxie@yzu.edu.cn
基金资助:
江苏省科技成果转化专项;江苏省科技支撑计划项目;江苏高校优势学科建设工程资助项目

Determination of Amoxicillin Residues in Eggs by HPLC with Fluorescence Detection

Received:2011-11-29 Revised:2012-10-19 Online:2012-11-25 Published:2012-11-20
Contact: Kai-Zhou XIE E-mail:kzxie@yzu.edu.cn

摘要/Abstract

摘要： 建立鸡蛋中阿莫西林残留的高效液相色谱荧光检测的方法。鸡蛋经乙腈提取，饱和二氯甲烷萃取，水杨醛酸性条件下沸水浴衍生化后，以0.01mol/L的磷酸二氢钾溶液(A)和乙腈溶液(B)为流动相，流速为1.0mL/min，荧光检测激发波长为354nm, 发射波长为445nm。阿莫西林在5.0～800ng/mL质量浓度范围内，本方法线性关系良好，相关系数为0.9997。当添加水平阿莫西林为5～125ng/g时，该方法平均回收率为80.47%～89.53%，相对标准偏差为5.77%～6.87%；日内相对标准偏差为8.61%～9.61%；日间相对标准偏差为11.01%～14.80%。阿莫西林检测限为1.2ng/g(RSN=3)、定量限为3.9ng/g(RSN=10)。所建立的方法简便、快速、灵敏度高，适用于鸡蛋中阿莫西林残留的高灵敏度检测。

关键词: 高效液相色谱, 荧光检测法, 阿莫西林, 鸡蛋, 残留

Abstract: An analytical method for the determination of moxicillin (AMO) residues in eggs was established using HPLC with fluorescence detection. AMO residues in egg samples were extracted with acetonitrile, and the acetonitrile extract was further extracted with saturated methylene chloride and derivatized with salicylaldehyde under acidic conditions in boiling water. The mobile phase used for the chromatographic separation of the derivative was composed of 0.01 mol/L potassium dihydrogen phosphate (A) and acetonitrile (B) at a flow rate of 1.0 mL/min. Fluorescence detection was completed at excitation and emission wavelengths of 354 nm and 445 nm, respectively. The HPLC method showed good linear relationship over the concentration range of 5.0–800 ng/mL (r = 0.9991). The average recoveries of AMO at spike concentrations between 5 ng/g and 125 ng/g were 80.47%–89.53% with a relative standard deviation (RSD) of 5.77%–6.87% and the intra-day and inter-day RSDs were 8.61%–9.61% and 11.01%–14.80%, respectively. The limit of detection and limit of quantification for AMO were 1.2 ng/g (RSN = 3) and 3.9 ng/g (RSN = 10), respectively (n = 6). This method was simple, fast, sensitive and suitable for the determination of AMO in eggs.

Key words: high performance liquid chromatography (HPLC), fluorescence detection, amoxicillin (AMO), eggs, residue

中图分类号:

S859.84

谢恺舟1,2，陈学森 1,2，徐?东1,2，郭辉生1,2 ，贾龙飞1,2 ，谢?星3，黄玉萍1,2，张小杰1,2，. 高效液相色谱荧光检测法检测鸡蛋中阿莫西林残留[J]. 食品科学, 2012, 33(22): 264-268.

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