超高效液相色谱法（UPLC）快速测定水产品中17种磺胺类抗生素残留

Rapid and simultaneous determination of seventeen sulfonamide residues in aquatic products by ultra performance liquid chromatography

中文关键词: 超高效液相色谱  水产品  磺胺  药物残留

英文关键词: Ultra Performance Liquid Chromatography (UPLC)  Aquatic products  Sulfonamides  Drug residue

中文摘要:

      采用超高效液相色谱（UPLC）—二极管阵列检测器（PDA），建立了水产品中17种磺胺类（SAs）抗生素残留的快速同时检测技术。样品经乙酸乙酯提取，HLB固相萃取柱净化，ACQUITY UPLCTM BEH C18色谱柱(2.1 mm×100 mm，1.7 μm)分离，以甲醇 0.1%乙酸为流动相，二极管阵列检测器（PDA）检测。17种磺胺在8 min内实现同时分离测定，磺胺类抗生素在0.01~5 μg/ml（磺胺醋酰、磺胺嘧啶和磺胺二甲异嘧啶为0.01～2 μg/ml）范围内线性关系良好（r≥0.999 8）。方法的检出限（S/N=3)为2.0~5.0 μg/kg，17种磺胺在添加水平分别为10、40 μg/kg时，平均回收率为70.4%～91.4％和73.3%～92.5％，相对标准偏差（RSD）小于10%。结果表明，该方法快速、灵敏、高效，适用于水产品中多种磺胺类抗生素的同时测定。

英文摘要:

      A method for the determination of 17 sulfonamides(SAs)in aquatic products by ultra performance liquid chromatography(UPLC)with photodiode array(PDA)detector was developed.The SAs in the samples were first extracted with ethyl acetate，then the ethyl acetate extraction was purified and concentrated by HLB cartridges.The analyses were performed on UPLC with an ACQUITY UPLC BEH C18column(2.1 mm×100 mm,1.7 μm),and the mobile phase was methanol 0.1％ acetic acid aqueous solution.SAs were separated by gradient elution and detected by PDA within 8 min.This method showed a good linearity.For sulfacetamide,sulfadiazine and sulfisomidine,the linearity was in the range of 0.01~2 μg/ml,and for the other SAs,the linearity ranged in 0.01~5 μg/ml.The detection limits of SAs were 2.0~5.0 μg/kg (S/N=3).At the spiked levels of 10 and 40μg/kg,the average recoveries of SAs were 70.4%～91.4％ and 73.3%～92.5％,respectively.The relative standard deviations were less than 10％.Routine tests show that the proposed separation and determination method is rapid,sensitive and efficient and indicate that it is practical for the determination of SAs in aquatic products.