摘要
试验旨在建立超高效液相色谱-串联质谱法(UPLC-MS/MS)测定风干的猪粪样品中氧氟沙星残留量。猪粪样品用0.1%甲酸乙腈(1∶9)提取和阳离子交换固相萃取小柱(MCX)净化后,以氧氟沙星-D8作为内标物,采用UPLC-MS/MS测定。结果显示,该方法在0.1~100.0μg/L范围内线性关系良好,方法最低检出限为3.5μg/kg,定量限为10.0μg/kg。在10、20、50μg/kg不同浓度的添加水平下,氧氟沙星的回收率在96.53%~110.45%之间,相对标准偏差在1.4%~11.1%之间。研究表明,该方法准确、灵敏、快捷,可作为猪粪中氧氟沙星残留的快速确证和定量分析方法。
The experiment aimed to establish a method for determining the residue of enrofloxacin in dried pig manure samples using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The experiment involved extracting pig manure samples with a 0.1%acetonitrile extraction solution(1∶9)and purifying them using a cation exchange solid-phase extraction cartridge(MCX).Enrofloxacin-D8 was used as an internal standard,and the determination was performed using UPLC-MS/MS.The results showed that the method had a good linear relationship in the range of 0.1 to 100.0μg/L,with a method detection limit of 3.5μg/kg and a quantification limit of 10.0μg/kg.At different spiking levels of 10,20 and 50μg/kg,the recovery rates of enrofloxacin ranged from 96.53%to 110.45%,and the relative standard deviations were between 1.4%and 11.1%.The study indicates that the method is accurate,sensitive,and rapid,and can be used for the rapid confirmation and quantitative analysis of enrofloxacin residues in pig manure.
作者
张婧
吴雨珊
王博
吴剑平
严凤
曹莹
ZHANG Jing;WU Yu-shan;WANG Bo;WU Jian-ping;YAN Feng;CAO Ying
出处
《饲料研究》
CAS
北大核心
2024年第20期125-128,共4页
Feed Research
基金
上海市农业科技创新项目(项目编号:2023-02-08-00-12-F04584)。