超高效液相色谱-串联质谱快速检测猪肉中的沃尼妙林残留  

Detection of Valnemulin Residues in Pork by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：于倩倩[1] 汪霞[2] 李一婧[3] 杨娟[4] 李秀波[4] 吴文学[1] 

机构地区：[1]中国农业大学动物医学院国家原虫实验室,北京100193 [2]中国兽医药品监察所,北京100081 [3]沈阳药科大学,沈阳110016 [4]中国农业科学院饲料所,北京100081

出　　处：《中国兽药杂志》2011年第4期24-27,共4页Chinese Journal of Veterinary Drug

摘　　要：建立了检测猪肉样品中新型兽药盐酸沃尼妙林残留的快速超高效液相色谱-串联质谱（UPLC-MS/MS）确证方法。样品使用乙腈提取,在提取过程中同时加入正己烷去除脂质杂质,离心后取乙腈提取液,浓缩至干,用1 mL 0.1%甲酸水∶乙腈（60∶40,V∶V）复溶上机。以反相C18柱作为分离柱,0.1%甲酸乙腈和0.1%甲酸水为流动相,进行梯度洗脱。方法的检测限为10μg/kg,定量限为20μg/kg;在三个浓度水平（20、50、100μg/kg）下进行添加实验,平均回收率均大于92.60%,批内相对标准偏差为1.31%~6.80%,批间相对标准偏差为3.02%~4.60%。此方法简便迅速且稳定有效,适合快速检测猪肌肉中的沃尼妙林残留。A method was developed for quantitative and qualitative determination of valnemulin（VLM） hydrochloride residue in porcine muscles by using ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）.The samples were extracted with acetonitrile at the same time adding hexane to remove the fat,then centrifuged and removed the hexane,just evaporated the part of acetonitrile.The residue was dissolved with acetonitrile-0.1% formic acid（40∶60,V∶V）.Chromatographic separation of the valnemulin was performed on a C18 column using formic acid 0.1% in acetonitrile and formic acid 0.1% in water by gradient elution.The LOD and LOQ of this method were 10 μg/kg and 20 μg/kg,respectively.Average analyte recoveries were more than 92.60% in replica sets of porcine muscles at three different concentrations（20、50、100 μg/kg）.Inter-day RSD was from 1.31% to 6.80%,and intra-day RSD was from 3.02% to 4.60%.The results suggested that this method was a robust and effective method for determination of valnemulin residues in pork.

关 键 词：沃尼妙林 超高效液相色谱-串联质谱 猪肉 残留 

分 类 号：S859.84[农业科学—临床兽医学]