Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1217, Issue 36, Pages 5724-5731Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2010.07.004
Keywords
Phenols; Soil; Simultaneous extraction; QuEChERS; Derivatization; GC-MS/MS
Funding
- Andalusian Regional Government [P07-AGR-02922]
- Spanish Ministry of Science and Innovation-European Social Fund, SMSI-ESF
- Ramon y Cajal Program (SMSI-ESF)
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Due to the different physico-chemical properties of phenols, the development of a methodology for the simultaneous extraction and determination of phenolic compounds belonging to several families, such as chlorophenols (CPs), alkylphenols (APs), nitrophenols (NTPs) and cresols is difficult. This study shows the development and validation of a method for the analysis of 13 phenolic compounds (including CPs, APs, NTPs and cresols) in agricultural soils. For this purpose, a quick, easy, cheap, effective, rugged and safe (QuEChERS)-based procedure was developed, validated and applied to the analysis of real samples. A derivatization step prior to the final determination by gas chromatography (GC) coupled to a triple quadrupole analyzer operating in tandem mass spectrometry (QqQ-MS/MS) was performed by using acetic acid anhydride (AAA) and pyridine (Py). The optimized procedure was validated, obtaining average extraction recoveries in the range 69-103% (10 mu g kg(-1)), 65-98% (50 mu g kg(-1)), 76-112% (100 mu g kg(-1)) and 76-112% (300 mu g kg(-1)), with precision values (expressed as relative standard deviation, RSD) <= 22% (except for 4-chlorophenol) involving intra-day and inter-day studies. Furthermore, 15 real soil samples were analyzed by the proposed method in order to assess its applicability. Some phenolic compounds (e.g. 2,4,6-trichlorophenol or 4-tert-octylphenol) were found in the samples at trace levels (<10 mu g kg(-1)). (C) 2010 Elsevier B.V. All rights reserved.
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