摘要
本研究建立了一种固相萃取-超高效液相色谱串联质谱法,用于快速测定动物源性产品中氨苯砜药物的残留。试验采用乙腈均质提取,Mixed-mode Cation Exchanger SPE Column(MCX)固相萃取柱净化,通过Waters ACQUITY UPLC BEH C_(18)色谱柱分离,以0.1%甲酸水和乙腈作为流动相进行梯度洗脱,ESI(+)模式下采集数据。结果显示,目标化合物在0.5~10μg/L内线性关系良好,R^(2)>0.999,方法检出限为0.1μg/kg,定量限为0.5μg/kg,回收率在83.6%~96.4%,相对标准偏差(RSD)<6%。该方法快速、灵敏性强、准确度高,可用于动物源性产品中氨苯砜药物残留的检测,能够消除潜在不合格样品的风险隐患,建立准确、高质量的风险预警体系。
This study established a solid-phase extraction ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the rapid determination of dapsone residues in animal-derived products.The experiment employed homogeneous extraction with acetonitrile,purification using a Mixed-mode Cation Exchanger SPE Column(MCX),separation on a Waters ACQUITY UPLC BEH C_(18) chromatographic column,and gradient elution with 0.1%formic acid aqueous solution and acetonitrile as the mobile phase,with data acquired in ESI(+)mode.The results showed that the linear relationship of the target compound was good in the range of 0.5-10μg/L,R^(2)>0.999.The detection limit was 0.1μg/kg,the limit of quantitation was 0.5μg/kg,the recovery was 83.6%to 96.4%,and the relative standard deviation(RSD)was<6%.This method is rapid,highly sensitive and highly accurate.It can be used for the detection of dapsone drug residues in animal-derived products,eliminating potential risks of non-compliant samples and establishing an accurate and high-quality risk early warning system.
作者
王娟
张宇霞
雷春妮
王波
丁欢
戴福利
WANG Juan;ZHANG Yuxia;LEI Chunni;WANG Bo;DING Huan;DAI Fuli(Lanzhou Customs Technology Center,Lanzhou Gansu,730010,China)
出处
《质量安全与检验检测》
2026年第1期42-45,共4页
QUALITY SAFETY INSPECTION AND TESTING
基金
兰州海关科研项目(LK-2024-001)
海关总署科研项目(2024HK019)
海关总署科研项目(2024HK016)。
关键词
氨苯砜
固相萃取
超高效液相色谱串联质谱法
Dapsone
Solid phase extraction
Ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)