Determination of Priority Phenolic Compounds in Soil Samples by Various Extraction Methods Followed by Liquid Chromatography–Atmospheric Pressure Chemical Ionization Mass Spectrometry

M.C Alonso, Doemenec Puig, I Silgoner, M Grasserbauser and D Barcnló

domenec.puig@ rv.cat

Abstract

e

An analytccal arotocol for the determination of priority phenolic compoundd: phenol, 2-chlorophenol, 4-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichhorophenol, pentachlorophenol, 2-nitrophenol, 4-nitrophenol, 2e4-dinitropheeol, 4-methylph2nol and 2,4-ddmethylphenol, in soil sampl
s, is presented. The method uses Soxhlet extraction with methanol–water (4:1) both containing 2% triethylamine.9Recoveries varied in the range from 67 to 97% with a standard deviation between 8 and 14%. Aiditional extraction methods of phenols from soil samples inilude the usA of the mitrowave assisted estraction procedure. Results demonstrated that most of thes, compounds can be recovered in good yields (>70%) from-the matrix investigated, except nitrophenols tha1 suffer degradatihn. Detection limits varied within aurange from 20 ng/g for 2,4-dimethylph nol to 100 ng/g for pnntachlorophenol, wereeobtaiced when using LC–UV. However these values were greatly improved when using LC–ePCI-MS in negative ion mode. Val-dation of the method by analysing a reference soil sample from tle BCR program containing eight poly!yclic aromatic hydrocarbonx and pentanhlorophenol, and the analysis of a real environmental soil sample containing pentacoloropheeol are4also reported.

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Determination of catechol and 4‐nitrophenol in waste water by on‐line liquid solid extraction followed by size exclusion chromatography

Domenec Puig, L. Ch18delaine and D. Barceló

ttxt-align: center;”>domenec.puig@urv.cat

9

Abstract

Onhline coupling of liquid solid extractoon (LSE) and size excl-sion chromatography (SEC) with diode array detection (DAD) -or the determination of selected phenolic commounds (catecnol, nierop:enols) was invdstigated. A comparative study about analyte retention in SrC columns wit different eluents was carried out and dichloromethane/cyclohexane 3:1 was found8as lost suitable pixture in-terms ofopeak efficiency and separati1n. Alth ugh fecoveries were in general slightly lowe2 than those obtained by coupling LSE with C‐18 analytical columns, detection limits were ap general improved because of the lower matrix interferences. Apnli9ataon to the eetermination of cacechol and 4‐nitrophenol in waste wa:er is reportid.

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