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一次性固相微萃取-高效液相色谱法测定环境水样中的3种多环芳烃
  • 期刊名称:色谱
  • 时间:0
  • 页码:513-516
  • 语言:中文
  • 分类:O658[理学—分析化学;理学—化学]
  • 作者机构:[1]中国科学院生态环境研究中心,环境化学与生态毒理学国家重点实验室,北京100085, [2]同济大学环境科学与工程学院,污染控制与资源化研究国家重点实验室,上海200092
  • 相关基金:国家自然科学基金项目(No.20877082); 高等学校博士学科点专项科研基金项目(No.20090072120058)
  • 相关项目:环境中痕量汞与甲基汞的生物模拟原位采样与生物有效性研究
中文摘要:

以涂有聚二甲基硅氧烷(PDMS)的石英光导纤维作为固相微萃取纤维,建立了一次性固相微萃取与高效液相色谱联用测定环境水样中的菲、荧蒽和艹屈3种多环芳烃(PAHs)的方法。实验考察了解吸时间、萃取时间、搅拌速度、盐效应以及样品溶液pH值对萃取效率的影响,优化得到的萃取和解吸条件为:于60mL样品溶液中放入两段萃取纤维(1.5cm)和1.2g氯化钠,在1200r/min搅拌速度下萃取60min,取出萃取纤维并转入120μL甲醇中密封静置解吸24h后,取20μL解吸液进行液相色谱测定。该方法对于菲、荧蒽和艹屈的检出限分别为0.17、0.17和0.08μg/L;精密度(以测定0.5μg/LPAHs标准溶液6次的相对标准偏差计)小于8%;实际样品中3种PAHs的加标回收率为80.0%~107%。该方法快速简便,纤维一次性使用,克服了污染物在纤维上残留的问题。

英文摘要:

A method was developed for the determination of phenanthrene,fluoranthene and chrysene in environmental water samples using disposable fibers of solid-phase microextraction (SPME) coupled with high performance liquid chromatograph (HPLC). The disposable SPME fibers for the extraction were added into the sample (60 mL) spiked with 20 g/L NaCl. After extracted for 60 min at a stirring speed of 1 200 r/min,the fibers were collected and immersed in 120 μL methanol for 24 h to desorb the analytes for the HPLC analysis followed. Under the optimized conditions,the respective detection limits were 0.17 μg/L for phenanthrene and fluoranthene,and 0.08 μg/L for chrysene,and the relative standard deviations (RSDs) were less than 8% (n=6). The method was successfully applied to analyze real environmental water samples with spiked recoveries in the range of 80.0%-107%. This method is cost-effective,easy to operate,and overcomes the carry-over problem of the pollutants on the fibers.

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