高效液相色谱-荧光检测同时测定污泥中7种氟喹诺酮类抗生素  

Simultaneous determination of seven fluoroquinolones in sewage sludge by high performance liquid chromatography with fluorescence detection

作　　者：陈莉 贾春虹[1] 刘冰洁[1] 靖俊杰 赵尔成[1] 余苹中[1] 贺敏[1] CHEN Li;JIA Chunhong;LIU Bingjie;JING Junjie;ZHAO Ercheng;YU Pingzhong;HE Min(Institute of Plant and Environment Protection,Beijing Academy of Agriculture and Forestry Sciences,Beijing 100097,China)

机构地区：[1]北京市农林科学院植物保护环境保护研究所

出　　处：《地学前缘》2019年第6期7-12,共6页Earth Science Frontiers

基　　金：国家重点研发计划项目(2017YFD0800900);国家自然科学基金项目(41101482);北京市自然科学基金项目(8122021)

摘　　要：为了监测污泥中氟喹诺酮类抗生素(FQs)的含量和水平,建立了基于固相萃取-高效液相色谱荧光检测法测定污泥中7种FQs的分析方法。污泥样品选用乙腈∶磷酸盐缓冲液(1∶1,V∶V)(pH=3)提取,以亲水亲油平衡(hydrophilic-lipophilic balance,HLB)小柱净化富集,经甲醇洗脱、浓缩后用高效液相色谱-荧光检测器(HPLC-FLD)检测,采用乙腈/0.1%的甲酸作为流动相并以外标法定量。FQs在0.005~1.0mg/L浓度范围内呈现良好线性关系,R2为0.9927~0.9998。添加量为0.05、0.5和1.0mg/kg时,污泥中7种氟喹诺酮类的加标回收率为78.3%~106.4%,其相对标准偏差为3.68%~12.06%(N=5)。方法的检出限为0.001~0.01mg/kg,方法定量限为0.0046~0.0384mg/kg。用该方法对北京地区3个污水处理厂活性污泥样品中7种FQs进行分析,检出浓度范围为未检出至1.09mg/kg。We have developed an analytical method for simultaneous determination of seven fluoroquinolones(FQs)in sewage sludge based on solid-phase extraction and high performance liquid chromatography with fluorescence detection(HPLC/FLD)in this study to monitor the FQ contents and levels in sewage sludge.The homogenized sludge sample was subjected to pH 3 phosphate buffer/acetonitrile(1∶1,V∶V)solution treatment,then loaded onto an Oasis HLB solid phase column after vortexing and eluted with methanol solvent.The FQs in the extract were detected by HPLC/FLD with acetonitrile and 0.1%formic acid as the mobile phase,and quantified using external standards.The standard curves for all the compounds were linear over the concentration ranges of 0.005 to 1.0 mg/L with R^2 equaling 0.9927-0.9998.The spiked recoveries at 0.05,0.5 and 1.0 mg/L levels ranged between 78.3%-106.4%,with relatives standard deviations(RSD)ranging between 3.68%-12.06%(N=5).The limit of detection(LOD)was between 0.001-0.01 mg/kg,and the limit of quantification(LOQ)ranged between 0.0046-0.0384 mg/kg.We used this method to analyze seven FQs in sewage sludge collected from three sewage treatment plants in Beijing.and found the FQ concentrations to be from ND to 1.09 mg/kg in tested samples.

关 键 词：氟喹诺酮类抗生素(FQs) 固相萃取-高效液相色谱荧光检测法(SPE-HPLC/FLD) 污泥 检测方法 

分 类 号：TQ450.2[化学工程—农药化工] X592[环境科学与工程—环境工程]