同位素内标-液质联用法测定鸡可食性组织中替米考星残留量  

Determination of Tilmicosin Residue in Edible Chicken Tissues by an Isotope-labeled Internal Standard Liquid Chromatography Tandem Mass Spectrometry

作　　者：蒋欣延 杨洁 袁聪 孟蕾 彭丽 吴宁鹏 JIANG Xin-yan;YANG Jie;YUAN Cong;MENG Lei;PENG Li;WU Ning-Peng(College of Veterinary Medicine,Henan Agricultural University,Zhengzhou 450002,China;Henan Provincial Research Institute of Agricultural,Animal and Fishery Products Inspection Technology,Zhengzhou 450008,China)

机构地区：[1]河南农业大学动物医学院,郑州450002 [2]河南省农畜水产品检验技术研究院,郑州450008

出　　处：《中国兽药杂志》2024年第5期26-33,共8页Chinese Journal of Veterinary Drug

摘　　要：建立了鸡四种可食性组织中替米考星的超高效液相色谱-串联质谱法。样品经磷酸二氢钾缓冲液和乙腈提取后,C_(18)固相萃取柱净化,以0.1%甲酸乙腈溶液和0.1%甲酸水为流动相,液相色谱-串联质谱法测定,内标法定量。试验结果表明:鸡四种可食性组织中替米考星在1~100μg/kg的浓度范围内呈线性关系,相关系数r大于0.99;替米考星在鸡四种可食性组织中的检测限为0.5μg/kg,定量限为1μg/kg;四种组织中替米考星添加浓度为1~4800μg/kg时,批间平均回收率为94.6%~100.9%,批内、批间变异系数在1.11%~5.06%范围之间。本方法适用于鸡四种可食性组织中替米考星含量的测定。A liquid chromatography tandem mass spectrometry(LC-MS/MS)internal standard method for the detection of tilmicosin in four chicken edible tissues has been established.The samples were extracted with potassium dihydrogen phosphate buffer and acetonitrile,then cleaned up by C_(18) solid phase extraction columns,with 0.1%formic acid acetonitrile 0.1%formic acid water as the mobile phase,and was determined by liquid chromatography tandem mass spectrometry and quantified by internal standard method.The experimental results showed that there was a good linear relationship between the concentration range of 1μg/kg to 100μg/kg of tilmicosin in four chicken edible tissues,and the correlation coefficient r was greater than 0.99.The detection limit of tilmicosin in four chicken edible tissues is 0.5μg/kg,and the quantitative limit is 1μg/kg,when the concentration of timicosin in four tissues is 1~4800μg/kg,the average batch-to-batch recovery rate is 94.6%~100.9%,the coefficient of variation within and between batches ranged from 1.11%to 5.06%.This method is suitable for the determination of tilmicosin content in four chicken edible tissues.

关 键 词：替米考星 鸡可食性组织 液相色谱-串联质谱法 内标法 

分 类 号：S859.84[农业科学—临床兽医学]