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OA
Simultaneous determination of sulfamethoxazole and its metabolites in pig manure by SPE-UPLC-MS/MS
本研究建立了固相萃取-超高效液相色谱串联质谱(SPE-UPLC-MS/MS)同步测定猪粪中磺胺甲噁唑及其7种代谢产物的方法,样本分别由McIlvaine-Na2EDTA缓冲液和有机混合固相萃取液逐次超声提取3次,再经固相萃取系统富集净化、经过氮吹、复溶过滤后,以甲醇和2 mmol/L甲酸铵为流动相进行UPLC-MS/MS分离检测.结果表明:1)在0.01～200 μg/L浓度范围内猪粪中磺胺甲噁唑及其7种代谢产物与对应峰面积呈良好的线性拟合关系,所有目标物标准曲线R2均大于0.99,检出限为0.004～0.017 μg/kg,定量限为0.18～0.51 μg/kg;2)在1、100、1000、10000 μg/kg 4个添加浓度下,8种目标化合物平均回收率为60.0％～99.7％,相对标准偏差为0.4％～5.0％,重复性及精准度良好;3)本方法适用于猪粪中磺胺甲噁唑及其7种代谢产物的同步测定,为猪粪中抗生素污染监测与风险评估提供了可靠分析方法.综上,该方法操作简单、灵敏度高,满足试验分析要求,可用于生猪粪便中SMX及其7种代谢产物残留的同时测定.
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.
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
农业农村部规划设计研究院农村能源与环保研究所/农业农村部资源循环利用技术与模式综合性重点实验室,北京 100121||黑龙江八一农垦大学工程学院,大庆 163319农业农村部规划设计研究院农村能源与环保研究所/农业农村部资源循环利用技术与模式综合性重点实验室,北京 100121中国农业大学资源与环境学院,北京 100193农业农村部规划设计研究院农村能源与环保研究所/农业农村部资源循环利用技术与模式综合性重点实验室,北京 100121||黑龙江八一农垦大学工程学院,大庆 163319农业农村部规划设计研究院农村能源与环保研究所/农业农村部资源循环利用技术与模式综合性重点实验室,北京 100121农业农村部规划设计研究院农村能源与环保研究所/农业农村部资源循环利用技术与模式综合性重点实验室,北京 100121农业农村部规划设计研究院农村能源与环保研究所/农业农村部资源循环利用技术与模式综合性重点实验室,北京 100121农业农村部规划设计研究院农村能源与环保研究所/农业农村部资源循环利用技术与模式综合性重点实验室,北京 100121本溪满族自治县连山关镇农业综合服务中心,辽宁本溪 117113
农业科技
猪粪磺胺甲噁唑代谢产物抗生素类药物残留
pig manuresulfamethoxazolemetabolitesantibiotic drug residues
《中国农业大学学报》 2026 (5)
129-142,14
国家重点研发计划课题(2024YFD1700703)农业农村部规划设计研究院自主研发项目(QD202418)
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