牛皮下注射爱普菌素注射剂后组织残留休药期的建立  

Development of Withdrawal Time of Eprinomectin Residue in Bovine Tissues after Subcutaneous Administration

作　　者：江海洋[1] 丁双阳[1] 刘金凤[1] 赵思俊[2] 何继红 吴聪明[1] 李建成[1] 沈建忠[1] 

机构地区：[1]中国农业大学动物医学院／国家兽药残留基准实验室,北京100193 [2]中国动物卫生与流行病学中心,青岛266032 [3]中牧实业股份有限公司,北京100070

出　　处：《畜牧兽医学报》2009年第3期444-450,共7页ACTA VETERINARIA ET ZOOTECHNICA SINICA

基　　金：“十一五”国家科技支撑计划课题(2006BAD31B08)

摘　　要：建立牛肌肉、肝脏、肾脏和脂肪组织中爱普菌素残留的高效液相色谱荧光检测方法（HPLC-FLD）,并用统计学方法计算牛皮下注射爱普菌素后组织残留的休药期。牛组织样品经乙腈提取,过碱性SPE柱。组织样品添加浓度为2～100 ng·g^-1,平均回收率为70.5%～91.2%,变异系数为2.3%～11.5%;方法检测限和定量限分别为1和2 ng·g^-1。18头牛颈部皮下一次性注射爱普菌素注射液（1%）,注射剂量为200μg.kg-1体质量,分别在给药后第1、3、7、14、21、28天各屠宰3头取样,经HPLC-FLD分析。结果表明,皮下单次注射给药后,肌肉中药物残留量（2.1～9.3 ng·g^-1）低于美国规定的残留限量（10 ng·g^-1）;肝脏中药物残留量（29.8～625.1 ng·g^-1）低于美国、欧盟和CAC规定的残留限量（分别为4 800、1 500和2 000 ng·g^-1）;肾脏和脂肪中药物残留量（4.1～112.5ng·g^-1和2.1～96.4 ng·g^-1）都低于欧盟和CAC规定的残留限量（300和250 ng·g^-1）。采用欧盟官方推荐方法对残留浓度-时间数据统计分析,牛肌肉、肝脏、肾脏、脂肪休药期均为0 d。In this study, a high performance liquid chromatography method with fluorescence detector （HPLC-FLD） was developed for determination of eprinomectin residue in bovine muscle, liver, kidney, and fat tissues. The tissue samples were extracted with acetonitrile, and cleaned up using basic SPE cartridge. Fortified at levels of 2-100 ng ·g^-1, mean recoveries were 70. 5%- 91.2%, with coefficient of variation of 2.3%-11.5%. The limit of detection and limit of quantiration were 1 and 2 ng ·g^- 1, respectively. Eighteen parasite-free cross cattle were treated with 1% eprinomectin injectable oil formulation at a dose rate of 0.2 ng·g^-1 body weight. Six batches of three treated animals （two males and one female） each were selected randomly at 1, 3, 7, 14, 21, and 28 days withdrawal after injection and the tissue （muscle, liver, kidney, and fat） samples were collected and analyzed by the above HPLC-FLD method. The results indicated that the residue concentration in muscle （2.1-9.3 ng·g^-1） was below the limit （10 ng·g^-1） approved by USA and the concentration in liver （29.8-625.1 ng·g^-1） was below the limits （4 800,1 500 and 2 000 ng·g^-1） recommended by USA, EU, and CAC, respectively. The levels of eprinomectin residues in kidney and fat （4.1-112.5 ng·g^-1 and 2.1-96.4 ng·g^-1） were less than the limits （300 and 250 ng·g^-1） regulated by EU and CAC. The withdrawal periods for all bovine tissues were zero days after the residue concentration-time data were analyzed using a statistical method recommended by Committee for Veterinary Medicinal Products （CVMP） of The European Agency for the Evaluation of Medicinal Products.

关 键 词：爱普菌素 高效液相色谱 牛 残留消除 休药期 

分 类 号：S859.84[农业科学—临床兽医学]