中国农业大学学报2026，Vol.31Issue(5)：129-142,14.DOI:10.11841/j.issn.1007-4333.2026.05.11
猪粪中磺胺甲噁唑及其代谢产物的SPE-UPLC-MS/MS同步检测方法研究
Simultaneous determination of sulfamethoxazole and its metabolites in pig manure by SPE-UPLC-MS/MS
摘要
Abstract
A method was developed for the simultaneous determination of sulfamethoxazole and its seven metabolites in pig manure by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry(SPE-UPLC-MS/MS).The samples were ultrasonically extracted three times by McIlvaine-Na2 EDTA buffer and organic mixed solid phase extraction solution,respectively.After enrichment and purification by solid phase extraction system,nitrogen blowing,re-solution and filtration,UPLC-MS/MS separation and detection were carried out with methanol and 2 mmol/L ammonium formate as mobile phase.The results showed that:1)In the concentration range of 0.01-200 μg/L,sulfamethoxazole and its seven metabolites in pig manure showed a linear relationship with the corresponding peak area.The standard curve R2 of all targets was greater than 0.99,the detection limit was 0.004-0.017 μg/kg,and the limit of quantitation was 0.18-0.51 μg/kg.2)The average recoveries of the eight target compounds at four spiked concentrations of 1,100,1000,10 000 μg/kg were 60.0％-99.7％,and the relative standard deviations were 0.4％-5.0％,the repeatability and accuracy were good.3)This method was suitable for the simultaneous determination of sulfamethoxazole and its seven metabolites in pig manure,and provides a reliable analysis method for the monitoring and risk assessment of antibiotic pollution in pig manure.In summary,the method is simple,sensitive and meets the requirements of experimental analysis.It can be used for the simultaneous determination of SMX and its seven metabolites residues in pig manure.关键词
猪粪/磺胺甲噁唑/代谢产物/抗生素类药物残留Key words
pig manure/sulfamethoxazole/metabolites/antibiotic drug residues分类
农业科技引用本文复制引用
付义琦,王健,李彦明,郭占斌,周海宾,丁京涛,徐鹏翔,马双双,宋玉刚..猪粪中磺胺甲噁唑及其代谢产物的SPE-UPLC-MS/MS同步检测方法研究[J].中国农业大学学报,2026,31(5):129-142,14.基金项目
国家重点研发计划课题(2024YFD1700703) （2024YFD1700703）
农业农村部规划设计研究院自主研发项目(QD202418) （QD202418）
