地学前缘 ›› 2019, Vol. 26 ›› Issue (6): 7-12.DOI: 10.13745/j.esf.sf.2019.10.1

• 土壤污染环境监测 • 上一篇    下一篇

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

陈莉，贾春虹，刘冰洁，靖俊杰，赵尔成，余苹中，贺敏   

  1. 北京市农林科学院 植物保护环境保护研究所, 北京 100097
  • 收稿日期:2019-06-12 修回日期:2019-06-28 出版日期:2019-11-30 发布日期:2019-11-30
  • 作者简介:陈莉(1973—)，女，博士，副研究员，主要从事土壤有机污染物的检测技术与污染防治研究。E-mail：chenli517@126.com
  • 基金资助:
    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)

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

CHEN Li，JIA Chunhong，LIU Bingjie，JING Junjie，ZHAO Ercheng，YU Pingzhong，HE Min   

  1. Institute of Plant and Environment Protection, Beijing Academy of Agriculture and Forestry Sciences, Beijing 100097, China
  • Received:2019-06-12 Revised:2019-06-28 Online:2019-11-30 Published:2019-11-30
  • Supported by:
     

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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0.005～1.0 mg/L浓度范围内呈现良好线性关系，R2为0.992 7～0.999 8。添加量为0.05、0.5和1.0 mg/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0.001～0.01 mg/kg，方法定量限为0.004 6～0.038 4 mg/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1.09 mg/kg。

 

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

Abstract: 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 R2 equaling 0.99270.9998. 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 0.0010.01 mg/kg, and the limit of quantification (LOQ) ranged between 0.00460.0384 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.

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