高效液相色谱-串联质谱法测定牛羊组织中苯酚类和水杨酸苯胺类抗蠕虫药多残留  

Simultaneous Determination of Phenolic and Salicylanilide Anthelmintics Multi-residues in Cattle and Ovine Tissues by HPLC-MS/MS

作　　者：李帅鹏[1] 黄显会[1] 王伟[1] 严常燕[1] 孔祥凯[1] 

机构地区：[1]华南农业大学国家兽药残留基准实验室,广州510642

出　　处：《分析化学》2014年第3期423-428,共6页Chinese Journal of Analytical Chemistry

基　　金：2012年农业行业标准制修订项目(No.201214148)资助

摘　　要：建立了高效液相色谱-串联质谱法同时测定牛、羊组织中硝碘酚腈、氯羟柳胺、氯氰碘柳胺、碘醚柳胺4种苯酚类和水杨酸苯胺类抗蠕虫药的多残留检测方法.样品用乙腈-丙酮（60∶40,V/V）（肌肉、肝脏和肾脏组织）或1％三乙胺乙腈（脂肪组织）超声提取,MAX阴离子固相萃取柱净化,液相色谱分离,采用多反应监测负离子模式对4种药物同时进行定性定量分析,在1～100μg/L范围内,4种药物与其对应峰面积的线性关系良好,相关系数均大于0.99.在牛、羊组织中的检出限（LOD）均为1μg/kg,定量限（LOQ）均为2.5 μg/kg.在LOQ、0.5倍最高残留限量（MRL）、MRL、2倍MRL添加水平下,4种药物的平均回收率在71％～112％之间,日内相对标准偏差（RSD）在1.1％～14.0％之间,日间RSD在6.4％～14.7％之间.采用本方法对市场上动物可食性组织进行抽样检测,共抽检40份样品,2份样品检测出苯酚类和水杨酸苯胺类抗蠕虫药残留.A high performance liquid chromatography-tandem mass spectrometric （HPLC-MS/MS）method was developed for the simultaneous determination of four phenolic and salieylanilide anthelmintics including nitroxinil, oxyelozanide, closantel and rafoxanide in cattle and ovine tissues. Muscle, liverand kidney were extracted with acetonitrile-acetone （60： 40, V/V）and fat with 1% triethylamine in acetonitrile, then the extract was purified with MAX solid-phase extraction column. Qualitative and quantitative analysiswas achieved by HPLC-MS/MS undernegative multiple reaction monitoring （MRM） mode. Good correlation coefficients were obtained （R〉0.99） in the concentration range of 1-100 μg/L. The limits of detection （LOD） and limits of qualification （LOQ） for the four compounds were 1 and 2.5 μg/kg, respectively. The mean recoveries at the four levels of LOQ, 0.5 maximum residue limit （MRL）, MRL, 2MRL were between 71% and 112%, with the intra-day relative standard deviation（ RSD） in the range of 1.1%-14.0% and inter-day RSD in the range of 6.4%- 14.7%. Forty samples from the market were analyzed with the method, only two samples were found to show phenolic and salicylanilide anthelmintics residues.

关 键 词：苯酚类和水杨酸苯胺类抗蠕虫药 牛羊组织 多残留 高效液相色谱-串联质谱 

分 类 号：TS251.7[轻工技术与工程—农产品加工及贮藏工程]