快速溶剂萃取-毛细管电泳法测定土壤和底泥中磺胺类药物残留

建立了一种快速溶剂萃取(ASE)-毛细管电泳检测土壤和底泥中磺胺类药物残留的新方法。通过优化ASE的萃取条件,选取甲醇为萃取剂,在70℃、10.3 MPa的条件下提取土壤和底泥样品中的磺胺类药物。毛细管电泳检测磺胺嘧啶,磺胺甲基嘧啶和磺胺间二甲氧基嘧啶的标准曲线具有良好的线性(r>0.999)。方法的定量限(LOQ,S/N=10)为0.056～0.070 mg/kg。日内相对标准偏差在0.4%～2.5%之间,日间相对标准偏差在1.2%～4.6%之间。3个加标水平0.100、0.625、2.50 mg/kg的平均回收率在82%～103%之间,RSD≦4.3%。方法已用于土壤和底泥样品前处理和磺胺类药物残留检测。

Determination of sulfonamide residues in soil and bottom sediment by accelerated solvent extraction-capillary electrophoresis

A new accelerated solvent extraction(ASE) capillary electrophoretic method was developed for the determination of sulfonamide residues in soil and bottom sediment.Sulfonamide residues were extracted with methanol at 70℃ under 10.3 MPa pressure in less than 25 min.The standard curves for determination of sulfadiazine(SDI),sulfamerazine(SMR) and sulfadimethoxine(SDIM) by the capillary electrophoretic method have good linearity(r>0.999).The method limits of quantification(LOQs) were 0.056～0.070 mg/kg.Intra-day and Inter-day precisions were 0.4%～2.5% and 1.2%～4.6%,respectively.The samples were spiked at 0.100,0.625 and 2.50 mg/kg,their average recoveries ranged from 82% to 103%,and relative standard deviations(RSDs) were ≦4.3%.The method has been applied to sample pretreatment and determination of sulfonamide residues in soil and bottom sediment.