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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。
A new method of rapid solvent extraction (ASE) -capillary electrophoresis to detect sulfonamides in soil and sediment was established. By optimizing the extraction conditions of ASE, methanol was selected as extractant to extract sulfonamides in soil and sediment samples at 70 ℃ and 10.3 MPa. The standard curve of sulfadiazine, sulfamerazine and sulfadimethoxine was good linearity (r> 0.999) by capillary electrophoresis. The limit of quantification (LOQ, S / N = 10) was 0.056 to 0.070 mg / kg. The relative standard deviations in the days ranged from 0.4% to 2.5%, and the relative standard deviations in the day ranged from 1.2% to 4.6%. The average recoveries of three spiked levels of 0.100, 0.625 and 2.50 mg / kg ranged from 82% to 103% with RSD ≦ 4.3%. Methods have been used for soil and sediment sample preparation and sulfa drug residue testing.