液相色谱串联质谱内标法测定鸡血浆中替米考星含量  

Determination of Tilmicosin Content in Chicken Plasma by Liquid Chromatography Tandem Mass Spectrometry Internal Standard Method

作　　者：闫隆娟 任子昱 李慧素 杨洁 袁聪 孟蕾 张盼盼 刘婷婷 吴志明 YAN Longjuan;REN Ziyu;LI Huisu;YANG Jie;YUAN Cong;MENG Lei;ZHANG Panpan;LIU Tingting;WU Zhiming(College of Veterinary Medicine,Henan Agricultural University,Zhengzhou,Henan 450002;Henan Institute of Agricultural,Animal and Aquatic Products Inspection and Testing Techonologies,Zhengzhou,Henan 450008)

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

出　　处：《中国家禽》2024年第7期67-73,共7页China Poultry

摘　　要：研究旨在建立测定鸡血浆中替米考星含量的液相色谱串联质谱内标法。试验采用甲醇-乙腈(1∶3)溶液提取鸡血浆中替米考星,以0.1%甲酸乙腈-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。结果显示:鸡血浆中替米考星在25~2 000 ng/mL浓度范围内呈线性关系,相关系数(r)大于0.999 9;替米考星在鸡血浆中的检测限为15 ng/mL,定量限为25 ng/mL,添加浓度为25~1 500 ng/mL时,批内平均回收率为96.5%~102.3%,批内、批间变异系数均小于3.2%。研究表明,建立的液相色谱串联质谱内标法前处理过程简单、快速,选择性好,灵敏度、准确度和精密度较高,适用于鸡血浆中替米考星含量的检测。The experiment was aimed to establish a liquid chromatography tandem mass spectrometry internal standard method to determine the content of tilmicosin in chicken blood plasma.The experiment used methanol acetonitrile(1∶3)solution to extract temicoxacin from chicken plasma and 0.1%formic acid acetonitrile-0.1%formic acid water as the mobile phase.It was determined by liquid chromatography tandem mass spectrometry,and quantified by internal standard method.The experimental results showed that there was a linear relationship between the concentration range of 25 to 2000 ng/mL of tilmicosin in chicken plasma,with a correlation coefficient(r)greater than 0.9999.The detection limit of tilmicosin in chicken plasma was 15 ng/mL,and the quantification limit was 25 ng/mL.When the concentration of tilmicosin added to chicken blood plasma was 25 to 1500 ng/mL,the average recovery rate within the batch was 96.5%to 102.3%,and the coefficient of variation within and between batches was less than 3.2%.It's indicated that the established liquid chromatography tandem mass spectrometry internal standard method had a simple and fast pre-treatment process,good selectivity,high sensitivity,accuracy and precision,and was suitable for the determination of tilmicosin content in chicken plasma.

关 键 词：替米考星 鸡血浆 液相色谱串联质谱法 内标法 

分 类 号：S859.7[农业科学—临床兽医学]