高效液相色谱荧光检测法检测鸡蛋中阿莫西林残留

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。%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.