高效液相色谱法测定水和土壤中磺胺类抗生素

Determination of Sulfonamides Antibiotics in Water and Soil Using High Performance Liquid Chromatography

建立了固相萃取(SPE)-高效液相色谱法(HPLC)同时测定水和土壤中5种磺胺类抗生素的分析方法。水样过滤后采用HLB固相萃取柱净化、富集;土样采用甲醇/EDTA-Mcllvaine缓冲液提取,LC-SAX和LC-18串联固相萃取小柱净化富集;采用高效液相色谱,以乙腈和0.01mol/LH3PH4作为流动相,于270nm波长处对样品进行检测。5种抗生素在水和土壤中的检出限分别为0.94～13.2ng/L和0.24～3.3μg/kg;加标回收率分别为81.0～105.5%和72.6%～85.3%。采集了不同菜地土壤和污水处理厂水样,用上述方法进行了检测,表明本方法对环境样品中磺胺类抗生素的检测是可行的,污水厂进水和菜地土壤中磺胺类抗生素总浓度分别为2.26～12.12ng/L和53.68～155.24μg/kg。

An analytical method was developed for the determination of sulfonamides antibiotics in soil and water.Water sample was purified and concentrated by HLB cartridge,while soil sample was firstly extracted by a mixture of methanol and EDTA-Mcllvaine buffer,then purified and concentrated by LC-SAX and LC-18 cartridges in tandem.Using acetonitrile and 0.01 mol/L phosphoric acid as the mobile phase,and 270 nm as the detective wavelength,the detective limitation values for 5 sulfonamides antibiotics in water and soil were obtained from 0.94 to 13.2 ng/L and from 0.24 to 3.30 μg/kg respectively.The recoveries were 72.6%-85.3% for soil samples and 81.6%-105.5% for water samples.The method was applied to determine the sulfonamides antibiotics in water samples from sewage treatment plants and soil samples from vegetable fields,Pearl River Delta,South China,that the total amounts of sulfonamides ranged from 2.26 to 12.12 ng/L in water samples and 53.68 to 155.2 μg/kg in soil samples respectively.