| 摘要: |
| 为探索鸡组织中氢溴酸常山酮残留量及其消除规律，选取25~30日龄AA肉鸡100只，体重约1.0 kg，按氢溴酸常山酮推荐剂量3 mg/kg给药。于最后一次给药后第0 d、6 h、1 d、2 d、3 d、5 d和8 d等每个时间点处死10只鸡，并采集每只鸡的胸肌、皮肤+脂肪、全肝和双肾，分别装入密封袋，做好标记-20℃保存。鸡组织试样经胰蛋白酶酶解，乙酸乙酯提取，正己烷脱脂，固相萃取净化，采用超高效液相色谱-串联质谱检测，外标法定量，并采用WT1.4软件处理，从而推算其休药期。结果表明：该方法检测限为1.5 μg/kg，定量限为5.0 μg/kg；4种组织的添加回收率为74.8%~91.1%，批内、批间变异系数均<11.5%；残留检测结果表明肌肉和皮肤+脂肪组织的休药期为0 d，肾脏组织的休药期为4 d，肝脏组织的休药期为5 d。因此，本研究中检测方法操作简单，灵敏度较高，可用于鸡组织中氢溴酸常山酮残留的检测和分析。考虑到饲养环境和个体差异等因素的影响，建议氢溴酸常山酮的休药期暂定为5 d。 |
| 关键词: AA肉鸡 氢溴酸常山酮 超高效液相色谱-串联质谱 残留消除 |
| DOI：10.11841/j.issn.1007-4333.2019.03.09 |
| 投稿时间：2018-04-12 |
| 基金项目:国家自然科学基金项目（31272604） |
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| Determination of halofuginone residue and its depletion in chicken tissue by UPLC-MS/MS |
|
SUN Xiaojuan, LIANG Xueyan, HAO Zuhui, LI Jiancheng
|
| (College of Veterinary Medicine, China Agricultural University, Beijing 100193, China) |
| Abstract: |
| The purpose of this research was to determinate the halofuginone residue and its depletion in chicken tissue.A total of 100 AA broilers aged 25-30 d and weighted about 1.0 kg were selected and fed with recommended halofuginone dosage of 3 mg/kg.Ten chickens of each timepoint were sampled at 0 d,6 h,1 d,2 d,3 d,5 d and 8 d after the last time administration.Their pectoral muscle,skin+fat,liver and kidney were then respectively collected and stored at -20 ℃.The samples were extracted with ethyl acetate after enzymatic hydrolysis of trypsin solution,degreased with n-hexane,and purified on solid phase extraction column.UPLC-MS/MS was used to detect the halofugimone residue.External standard method was used for quantitative analysis,and the data of the residues were processed using WT1.4 software to calculate the withdrawal time.The results showed that:The detection limit and quantitative limit of this method were 1.5 and 5.0 μg/kg,respectively.The recovery rates of these four different tissues were ranged from 74.8% to 91.1%,and the coefficients of variation were less than 11.5%.The residues test results showed that withdrawal time was 0 d for muscle and skin+fat tissues,4 d for kidney and 5 d for liver.In conclusion,this method was simple for operation with higher sensitivity,and could be used for the detection and analysis of halofuginone residues in chicken tissues.Considering the influence of environment and individual differences,the withdrawal period of halofuginone was determined 5 d tentatively. |
| Key words: AA broilers halofuginone UPLC-MS/MS residue elimination |
