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固相萃取/固相微萃取-气相色谱法测定饮用水中多溴联苯醚

何迎春 王正虹 李林 周倩如

食品科学2012,Vol.33Issue(8):236-240,5.
食品科学2012,Vol.33Issue(8):236-240,5.

固相萃取/固相微萃取-气相色谱法测定饮用水中多溴联苯醚

Determination of Polybrominated Diphenyl Ethers in Drinking Water by Solid Phase Extraction or Solid-phase Micro-extraction Combined with Gas Chromatography

何迎春 1王正虹 2李林 1周倩如2

作者信息

  • 1. 西南大学食品科学学院,重庆400716
  • 2. 重庆市疾病预防控制中心,重庆400042
  • 折叠

摘要

Abstract

Objective: To establish a novel method for determining the contents of polybrominated diphenyl ethers(BDE-47 and BDE-99) in drinking water by solid phase extraction(SPE) or solid phase micro extraction(SPME) combined with gas chromatography(GC).Methods: In the SPE-GC method,100 mL of water sample was purified by LC-C18 SPE column chromatography through elution with hexane.The eluent was evaporated to dryness in water bath at 80℃,and the remaining residue was re-dissolved with isooctane and made up to 1 mL.Finally,1μL of the solution was injected into GC for the determination.The limits of detection(LOD) for BDE-47 and BDE-99 were 0.0008μg/L and 0.0009μg/L(RSN= 6),respectively,the regression equations showed good linearity with a correlation coefficient of 0.9996 and 0.9997,respectively,and the RSDs for 6 replicate determinations were in the range of 1.0%-4.9% and 0.96%-4.4%,respectively.In the SPME-GC method,10 mL of water sample was placed into a 15-mL SPME bottle and adsorbed by solid-phase micro-extraction for 25 min at 40 ℃ with a rotation speed of 1150 r/min.Then,the fiber was air-dried,immediately followed by GC analysis.The LODs of the SPME-GC method for BDE-47 and BDE-99 were 0.0000μg/L and 0.0044μg/L(RSN = 6),respectively,the linear correlation coefficients were 0.9996 and 09992,respectively,and the RSDs for 6 replicate determinations varied in the range of 6.7%-11.4% and 6.0%-10.1%,respectively.Results: BDE-47 and BDE-99 were undetected in 52 samples randomly collected from a certain city.Conclusion: Both analytical methods are characterized by simplicity,rapidity,high precision,good accuracy and satisfactory recovery rate.

关键词

固相萃取/固相微萃取/气相色谱/多溴联苯醚/饮用水

Key words

solid phase extraction/solid phase micro-extraction/gas chromatography/polybrominated diphenyl ethers/drinking water

分类

医药卫生

引用本文复制引用

何迎春,王正虹,李林,周倩如..固相萃取/固相微萃取-气相色谱法测定饮用水中多溴联苯醚[J].食品科学,2012,33(8):236-240,5.

食品科学

OA北大核心CSCDCSTPCD

1002-6630

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