摘要
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后,以0.01mol.L-1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-1,荧光检测激发波长为354nm,发射波长为445nm,建立了用高效液相色谱荧光法检测鸡蛋中氨苄西林残留的方法。氨苄西林在5.0～800.0μg.L-1,本方法线性关系良好,相关系数为0.999 4。当氨苄西林添加水平为5～125ng.g-1时,该方法平均回收率为78.30%～85.11%,相对标准偏差为4.99%～7.25%;日内相对标准偏差为7.99%～9.64%;日间相对标准偏差为8.69%～12.48%。氨苄西林检测限为0.4ng.g-1(S/N=3),定量限1.5ng.g-1(S/N=10)。所建立的方法简便、快速、灵敏度高,适用于鸡蛋中氨苄西林残留的高灵敏度检测。
A high performance liquid chromatography with fluorescence detection（HPLC-FLD） method was built for determination of residues of ampicillin（AMP） in eggs of laying hens. AMP was extracted in acetonitrile and saturat- ed methylene chloride from eggs. The extract solution was reacted to salicylide under acidic and heating conditions. The analysis was carried out using 0.01 mol/L potassium dihydrogen phosphate（A） and acetonitrile（B） as the mobile phase,the flow rate was 1. 0 mL · min-1. Fluorescence detection was carried out at excitation and emission wavelengths of 354 nm and 445 nm. The data indicated that the linear relationship of AMP was nice（r=0. 999 4） in 5.0 μg · L^-1 to 800.0μg · L^-1 concentration range. At spiked level of 5-125 ng · L^-1 for AMP,the average recovery ranged from 78. 30% to 88. 11 %, relative standard deviation（RSD） ranged from 4. 99% to 7. 25%, the intra-day RSD ranged from 7.99% to 9. 64% ,the inter day RSD ranged from 8.69% to 12. 48%. Limits of detection（LODs） were 0.4 ng · L^-1 （S/N=3） and limits of quantitation（LODs） was 1.5 ng · L^-1 （S/N：10） for AMP. This HPLC- FLD method is simple,rapid,high sensitivity and suitable for the determination of AMP in eggs of laying hens.
出处
《中国兽医学报》
CAS
CSCD
北大核心
2012年第8期1181-1185,共5页
Chinese Journal of Veterinary Science
基金
江苏省高新技术计划资助项目(BG2005307)
江苏省科技成果转化专项资助项目(BA2008071)
关键词
高效液相色谱
氨苄西林
鸡蛋
药物残留
high performance liquid chromatography（HPLC）
ampicillin（AMP）
eggs of laying hens
drugs residues
