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固相萃取-高效液相色谱-荧光检测土壤中喹诺酮类抗生素
引用本文:邰义萍,莫测辉,李彦文,包艳萍,张艳,姚圆,罗晓栋.固相萃取-高效液相色谱-荧光检测土壤中喹诺酮类抗生素[J].分析化学,2009,37(12).
作者姓名:邰义萍  莫测辉  李彦文  包艳萍  张艳  姚圆  罗晓栋
作者单位:1. 暨南大学环境工程系,广州,510632
2. 暨南大学环境工程系,广州,510632;暨南大学水生生物研究所,广州,510632
基金项目:国家自然科学基金项目,广东省自然科学基金重点项目,广东省科技计划项目,东莞市科技计划项目 
摘    要:建立了固相萃取-高效液相色谱-荧光(HPLC-FLD)检测土壤中4种喹诺酮类抗生素的分析方法.样品采用50% Mg(NO_3)_2-10% NH_3 · H_2O(96∶ 4,V/V)超声提取,过HLB柱富集净化,再用乙腈-0.067 mol/L H_3PO_4溶液洗脱.采用高效液相色谱-荧光检测器,以乙腈-0.067 mol/L H_3PO_4(用三乙胺调节至pH 2.5)为流动相,于激发波长280 nm、发射波长450 nm处进行检测.土壤样品中4种喹诺酮类抗生素的加标回收率在60.4%~99.3%之间,检出限为0.58~1.0 μg/kg.对蔬菜基地土壤样品分析结果表明,本方法能够满足实际样品的分析要求,4种喹诺酮类抗生素均被检出,土壤中抗生素污染问题值得关注.

关 键 词:土壤  喹诺酮类抗生素  固相萃取  高效液相色谱  荧光检测

Determination of Quinolones in Soils Using Solid Phase Extraction and High Performance Liquid Chromatography-Fluorimetric Detection
TAI Yi-Ping,MO Ce-Hui,LI Yan-Wen,BAO Yan-Ping,ZHANG Yan,YAO Yuan,LUO Xiao-Dong.Determination of Quinolones in Soils Using Solid Phase Extraction and High Performance Liquid Chromatography-Fluorimetric Detection[J].Chinese Journal of Analytical Chemistry,2009,37(12).
Authors:TAI Yi-Ping  MO Ce-Hui  LI Yan-Wen  BAO Yan-Ping  ZHANG Yan  YAO Yuan  LUO Xiao-Dong
Institution:TAI Yi-Ping1,MO Ce-Hui1,LI Yan-Wen1,2,BAO Yan-Ping1,ZHANG Yan1,YAO Yuan1,LUO Xiao-Dong1 (Department of Environment Engineering1,Institute of Hydrobiology2,Jinan University,Guangzhou 510632)
Abstract:An analytical method for the simultaneous determination of four quinolones in soil was developed. Soil samples were extracted by a mixture of 50% magnesium nitrate and 10% ammonia(96∶ 4, V/V)with an ultrasonic-assisted extraction, then purified and concentrated by HLB cartridge, and eluted with acetonitrile and 0.067 mol/L phosphoric acid(5∶ 1, V/V). Using acetonitrile and 0.067 mol/L phosphoric acid(pH=2.5) as the mobile phase, these analytes were quantificated by HPLC(fluorimetric detector) at excitation and emission wavelength of 280 nm and 450 nm respectively. The detective limits for four quinolones in soil were from 0.58 to 0.03 g/kg. The recoveries were 60.4% to 99.3% for soil samples. The method was successfully applied to determine the quinolones in soil samples from vegetable fields. Four quinolone compounds were detected to a different extent with total amounts of quinolones ranged from 27.84 to 129.26 μg/kg.
Keywords:Soil  quinolones  solid phase extraction  high performance liquid chromatography  fluorimetric detection
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