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优化离心固相萃取法测定水中 16 种多环芳烃

Optimization of a solid-phase extraction method using centrifugation for the determination of 16 polycyclic aromatic hydrocarbons in water.

机构信息

National Council for Scientific Research, Lebanese Atomic Energy Commission, Beirut, Lebanon.

出版信息

J Agric Food Chem. 2011 Jul 27;59(14):7592-600. doi: 10.1021/jf200123v. Epub 2011 Apr 18.

Abstract

A fast and reliable method for the determination of polycyclic aromatic hydrocarbons (PAHs) in water samples by solid-phase extraction (SPE) using centrifugation has been developed and optimized. A silica-based C18 cartridge was used; parameters affecting the extraction procedure such as type and volume of the elution solvent, breakthrough volume of the percolated water sample, drying of the sorbent, and evaporation of the elute have been studied. The innovation of this work was the examination of the use of a centrifugation technique in both the drying and elution steps. When combined with centrifugation, the volume of the elution solvent was reduced to 1 mL and the time for sorbent drying decreased also to 10 min under vacuum. Under optimal conditions, recoveries for the 16 U.S. EPA PAHs were between 70 and 85% and the relative standard deviation varied between 1 and 14%. Surrogate standard recoveries were similarly between 61 and 94% with a relative standard deviation between 2 and 15%. The simplicity of the described method, use of less of organic solvent, short procedure time, and good recoveries demonstrate the advantages of this environmentally friendly approach for routine analysis of numerous samples.

摘要

已经开发并优化了一种使用离心固相萃取(SPE)快速可靠地测定水样中多环芳烃(PAHs)的方法。使用基于硅胶的 C18 小柱;研究了影响萃取过程的参数,如洗脱溶剂的类型和体积、渗滤水样的穿透体积、吸附剂的干燥和洗脱液的蒸发。这项工作的创新之处在于考察了离心技术在干燥和洗脱步骤中的应用。当与离心结合使用时,洗脱溶剂的体积减少到 1 mL,真空下吸附剂干燥的时间也减少到 10 min。在最佳条件下,16 种美国环保署 PAHs 的回收率在 70%至 85%之间,相对标准偏差在 1%至 14%之间。替代标准的回收率也相似,在 61%至 94%之间,相对标准偏差在 2%至 15%之间。该方法简单,有机溶剂用量少,程序时间短,回收率高,证明了这种环保方法在常规分析大量样品方面的优势。

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