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固相萃取-高效液相色谱-串联质谱法同时测定土壤中氟喹诺酮、四环素和磺胺类抗生素
引用本文:马丽丽,郭昌胜,胡伟,沙健,朱兴旺,阮悦斐,王玉秋.固相萃取-高效液相色谱-串联质谱法同时测定土壤中氟喹诺酮、四环素和磺胺类抗生素[J].分析化学,2010,38(1).
作者姓名:马丽丽  郭昌胜  胡伟  沙健  朱兴旺  阮悦斐  王玉秋
作者单位:南开大学环境科学与工程学院环境污染控制过程与基准教育部重点实验室,天津,300071
基金项目:国家环境保护部全国饮用水源地基础环境调查及评估专项基金(No.2008AW01)资助项目
摘    要:建立了固相萃取-高效液相色谱-串联质谱法同时检测土壤中氟喹诺酮类、四环素类和磺胺类18种抗生素的分析方法。土样经含50%乙腈的磷酸盐缓冲液(pH=3)提取后,以SAX-HLB串联小柱净化富集,在HPLC/MS/MS多反应监测模式下进行定性及定量分析。添加浓度为200和50μg/kg时,土壤中氟喹诺酮类、四环素类、磺胺类的加标回收率分别为67.2%~89.0%,62.2%~85.4%和55.8%~97.4%;其相对标准偏差为1.1%~17.2%。以3倍信噪比估算出氟喹诺酮类、四环素类、磺胺类的检出限分别为3.4~8.9μg/kg,0.56~0.91μg/kg和0.07~1.85μg/kg。应用此方法检测6种不同类型土壤样品,结果表明,污灌区土壤中检出有抗生素,浓度为1.72~119.6μg/kg。

关 键 词:氟喹诺酮  四环素  磺胺  固相萃取  高效液相色谱串联质谱  土壤  

Simultaneous Extraction and Determination of Eighteen Fluoroquinolone, Tetracycline and Sulfonamide Antibiotics from Soils Using Solid-phase Extraction and Liquid Chromatography Tandem Mass Spectrometry
MA Li-Li,GUO Chang-Sheng,HU Wei,SHA Jian,ZHU Xing-Wang,RUAN Yue-Fei,WANG Yu-Qiu.Simultaneous Extraction and Determination of Eighteen Fluoroquinolone, Tetracycline and Sulfonamide Antibiotics from Soils Using Solid-phase Extraction and Liquid Chromatography Tandem Mass Spectrometry[J].Chinese Journal of Analytical Chemistry,2010,38(1).
Authors:MA Li-Li  GUO Chang-Sheng  HU Wei  SHA Jian  ZHU Xing-Wang  RUAN Yue-Fei  WANG Yu-Qiu
Institution:Key Laboratory of Pollution Processes and Environmental Criteria of Ministry of Education;College of Environmental Science and Engineering;Nankai University;Tianjin 300071
Abstract:An analytical method was developed for the simultaneous extraction and determination of eighteen fluoroquinolones (FQs),tetracyclines (TCs) and sulfonamides (SAs) antibiotics from soils using solid phase extraction and liquid chromatography tandem mass spectrometry.Soil sample was firstly extracted by phosphate buffer at pH 3 in combination with 50% of organic modifier acetonitrile,then purified and concentrated by SAX and HLB column.Qualitative and quantitative analysis were carried out for the analyte und...
Keywords:Fluoroquinolones  Tetracyclines  Sulfonamides  Solid phase extraction  High performance liquid chromatography-tandem mass spectrometry  Soil  
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