| 高效液相色谱荧光检测法检测鸡蛋中氨苄西林残留 |
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| 引用本文： | 谢恺舟,郭辉生,徐东,贾龙飞,谢星,陈学森,黄玉萍,张小杰,孙瑛瑛,王金玉.高效液相色谱荧光检测法检测鸡蛋中氨苄西林残留[J].兽医大学学报,2012(8):1181-1185. |
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| 作者姓名： | 谢恺舟 郭辉生 徐东 贾龙飞 谢星 陈学森 黄玉萍 张小杰 孙瑛瑛 王金玉 |
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| 作者单位： | [1]扬州大学动物科学与技术学院,江苏扬州225009 [2]江苏省动物遗传繁育与分子设计重点实验室,江苏扬州225009 [3]南京农业大学动物医学院,江苏南京210095 |
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| 基金项目： | 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） |
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| 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。
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| 关 键 词： | 高效液相色谱 氨苄西林 鸡蛋 药物残留 |
Determination of residues of ampicillin in eggs of laying hens by HPLC with fluo- rescence detection |
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| Authors: | XIE Kai-zhou ＇ GUO Hui-sheng XU Dong ＇ JIA Long-fei ＇ XIE Xing CHEN Xue-sen ＇ HUANG Yu-ping ＇ ZHANG Xiao-jie SUN Ying-ying WANG Jin-yu |
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| Institution: | 1＇2 (1. College of Ani- mal Science and Technology ,Yangzhou University ,Yangzhou , Jiangsu 225009, China ; 2. Key La- boratory for Animal Genetic ,Breeding,Reproduction and Molecular Design of J iangsu Province, Yangzhou ,Jiangsu 225009, China ; 3. College of Veterinary Medicine, Nanjing Agricultural Uni- versity, Nanj ing 210095, China) |
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| Abstract: | 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. |
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| Keywords: | high performance liquid chromatography（HPLC） ampicillin（AMP） eggs of laying hens drugs residues |
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