固相萃取-超高效液相色谱串联质谱法测定水产品中磺胺类药物残留

Determination of sulfonamide drugs residues in aquatic product by solid phase extraction-ultra performance liquid chromatography tandem mass spectrometry

目的建立同时测定水产品中磺胺嘧啶(sulfadiazine, SDZ)、磺胺甲恶唑(sulfamethoxazole, SMZ)、磺胺二甲嘧啶(sulfadimidine, SDM)、磺胺间甲氧嘧啶(sulfamonomethoxine, SMM)4种磺胺类药物残留的固相萃取-超高效液相色谱-串联质谱的检测方法。方法样品采用乙腈-0.2%甲酸溶液均质振荡提取,用CaptivaEMR-Lipid固相萃取柱净化,外标法定量。结果 4种磺胺类药物的检出限为0.08～0.12μg/kg,定量限为0.25～0.50μg/kg,回收率均为70.2%～103.4%之间。结论该方法具有基质干扰小、准确,易操作等优点,适用于水产品中4种磺胺类残留药物的检测。

Objective To establish a method for the determination of 4 kinds of sulfonamide drugs(sanodiazine,sulfamethoxazole,sulfadimidine and sulfamonomethoxine)residues in aquatic product by solid phase extraction-ultra performance liquid chromatography tandem mass spectrometry.Methods Samples were extracted with 0.2%formic acid acetonitrile solution,and the extract was purified on Captiva EMR–lipid solid phase extraction column.Quantification of the analytes was achieved by UPLC-MS using the external standard method.Results The results showed that the limits of detection(LODs)of 4 sulfonamide were in range of 0.08-0.12μg/kg and the limits of quantification(LOQ)were in range of 0.25-0.50μg/kg.The average recoveries of 4 sulfonamide drugs were from 70.2%to 103.4%.Conclusion This method has the advantages of low matrix interference,accuracy and easy operation,which is suitable for the detection of 4 kinds of sulfonamides residues in aquatic products.