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HERO ID
3605122
Reference Type
Journal Article
Title
Miniscale Liquid-Liquid Extraction Coupled with Full Evaporation Dynamic Headspace Extraction for the Gas Chromatography/Mass Spectrometric Analysis of Polycyclic Aromatic Hydrocarbons with 4000-to-14 000-fold Enrichment
Author(s)
Liew, CS; Li, X; Lee, HK
Year
2016
Is Peer Reviewed?
Yes
Journal
Analytical Chemistry
ISSN:
0003-2700
EISSN:
1520-6882
Publisher
AMER CHEMICAL SOC
Location
WASHINGTON
Volume
88
Issue
18
Page Numbers
9095-9102
Language
English
PMID
27535573
DOI
10.1021/acs.analchem.6b02056
Web of Science Id
WOS:000384038400024
Abstract
A new sample preparation approach of combining a miniscale version of liquid-liquid extraction (LLE), termed miniscale-LLE (msLLE), with automated full evaporation dynamic headspace extraction (FEDHS) was developed. Its applicability was demonstrated in the extraction of several polycyclic aromatic hydrocarbons (PAHs) (acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, and pyrene) from aqueous samples. In the first step, msLLE was conducted with 1.75 mL of n-hexane, and all of the extract was vaporized through a Tenax TA sorbent tube via a nitrogen gas flow, in the FEDHS step. Due to the stronger π-π interaction between the Tenax TA polymer and PAHs, only the latter, and not n-hexane, was adsorbed by the sorbent. This selectivity by the Tenax TA polymer allowed an effective concentration of PAHs while eliminating n-hexane by the FEDHS process. After that, thermal desorption was applied to the PAHs to channel them into a gas chromatography/mass spectrometric (GC/MS) system for analysis. Experimental parameters affecting msLLE (solvent volume and mixing duration) and FEDHS (temperature and duration) were optimized. The obtained results achieved low limits of detection (1.85-3.63 ng/L) with good linearity (r(2) > 0.9989) and high enrichment factors ranging from 4200 to 14 100. The optimized settings were applied to the analysis of canal water sampled from an industrial area and tap water, and this methodology was compared to stir-bar sorptive extraction (SBSE). This innovative combined extraction-concentration approach proved to be fast, effective, and efficient in determining low concentrations of PAHs in aqueous samples.
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