CAJ | 학술논문

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.
건립료고상췌취-고효액상색보-형광(HPLC-FLD)검측토양중4충규낙동류항생소적분석방법.양품채용50% Mg(NO_3)_2-10% NH_3 · H_2O(96∶ 4,V/V)초성제취,과HLB주부집정화,재용을정-0.067 mol/L H_3PO_4용액세탈.채용고효액상색보-형광검측기,이을정-0.067 mol/L H_3PO_4(용삼을알조절지pH 2.5)위류동상,우격발파장280 nm、발사파장450 nm처진행검측.토양양품중4충규낙동류항생소적가표회수솔재60.4%～99.3%지간,검출한위0.58～1.0 μg/kg.대소채기지토양양품분석결과표명,본방법능구만족실제양품적분석요구,4충규낙동류항생소균피검출,토양중항생소오염문제치득관주.
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.