摘要
建立一种测定牛肌肉组织中加米霉素残留的高效液相色谱-串联质谱方法。均质后的样品经0.1 mol/L磷酸二氢钾溶液提取,正己烷脱脂,HLB固相萃取柱净化,反相C 18色谱柱分离,采用多反应监测正离子模式测定。结果显示,该方法检测限为0.5μg/kg,定量限为2μg/kg;在2-400μg/kg范围内线性良好,相关系数r均大于0.999;平均回收率范围为91.6%-118.7%,批内变异系数在2.06%-11.06%之间(n=6),批间变异系数在3.86%-7.98%之间(n=18)。该方法灵敏、准确、重复性好,适用于牛肌肉组织中加米霉素残留量的测定。
The aim of the study was to establish a method for determination of gamithromycin residues in bovine muscle tissues by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Homogenized samples were extracted by 0.1mol/L potassium dihydrogen phosphate solution,degreased by n-hexane,purified by HLB solid phase extraction column,separated by reversed-phase C 18 column,then determined by multi-reaction monitoring positive ion mode.Results showed that LOD is 0.5μg/kg,LOQ 2μg/kg;Gamithromycin had good linear relationship in the range of 2-400μg/kg,and the correlation coefficient r is greater than 0.99;The average recovery was 91.6%-118.7%,the intra-assay coefficient of variation was 2.06%-11.06%(n=6),and the inter-assay coefficient of variation was 3.86%-7.98%(n=18).The results showed that the method was sensitive,accurate and reproducible,and was suitable for the determination of gamithromycin residues in bovine muscle tissue.
作者
伍宏凯
刘佩怡
刘燕
吴荔琴
肖田安
黄显会
WU Hongkai;LIU Peiyi;LIU Yan;WU Liqin;XIAO Tianan;HUANG Xianhui(Guangdong agriculture products quality and safety center,Guangzhou Guangdong 510230;National Reference Laboratory of Veterinary Drug Residues,South China Agricultural University,Guangzhou Guangdong 510642)
出处
《广东畜牧兽医科技》
2023年第6期50-54,共5页
Guangdong Journal of Animal and Veterinary Science