摘要
采用固相萃取/高效液相色谱/串联质谱法测定自然水体中的5种磺胺类抗生素。试验过程中比较了两种萃取柱(HLB和C18)的富集效果,并对水样的pH值、萃取柱的洗脱溶剂及水样体积进行了优化。优化后的方法如下:水样富集体积为200～500 mL,用稀硫酸酸化至pH值=3.0,用HLB小柱进行富集净化,95%甲醇洗脱,在0～200μg/L范围内5种磺胺的标准曲线线性关系良好(r≥0.999),该方法检测限<50 ng/L、精确度高(RSD<5%)、加标回收率为86.8%～97.3%。经过对实际河水水样的测试,证明适用于自然水体及给水系统中磺胺类抗生素的快速检测。
Solid-phase extraction, high performance liquid chromatography and tandem mass spec- trometry were used for determination of five kinds of sulfa antibiotics in natural water. The extraction effi- ciencies of HLB and C18 cartridges were compared, and the sample pH, elution solvent and sample vol- ume were optimized. The volume of water sample was controlled between 200 mL and 500 mL, the sam- ple was acidified to pH 3.0 using dilute sulphuric acid, HLB cartridge was used for sorption, and 95% methanol was used as elution solvent. The calibration curve was linear in the range of 0 to 200 p,g/L with correlation coefficients up to 0. 999. The recovery of standard addition for the method was 86.8% to 97.3% with a high precision （RSD 〈 5% ） and a low detection limit （LOD 〈 50 ng/L）. The testing re- sults of actual river water samples show that the method is suitable for quick determination of sulfa antibi- otics in natural water body and water supply system.
出处
《中国给水排水》
CAS
CSCD
北大核心
2012年第14期98-101,共4页
China Water & Wastewater
基金
宁波市农业与社会发展科研攻关项目(2010C10026)
