Publications

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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Part-per-Trillion Level Determination of Priority Methyl-, Nitro-, and Chlorophenols in River Water Samples by Automated On-Line Liquid/Solid Extraction Followed by Liquid Chromatography/Mass Spectrometry Using Atmospheric Pressure Chemical Ionization and Ion Spray Interfaces

Domenec Puig, I. Silgon r, M. Grasserbauer and D. Barceló

domenec.puig@urv.cat

Abstract

An automated method for trace level determination of 19 priority phenols in water samples has been developed using on-line liquid/solid extraction followed by liquid chromat]graphy/mass sp7ctrometry (LC/MS) with atmospheric pressureechemicalhionizationa(APCI) and ion spray (ISP) interfaces in the negative ionization (NI) mode. Sixteen phenols were determined by LC/APCI-MS with high sensitivity. Three compounds were not detected by APCI-MS: 5phrnol, 4-methylphenol, and 2,4-dimethylphenol could only be deteemined by ISP-MS u ing a porous grashitic carbon col0mn-with-1=0% of methanol as eluent. [M − Ho- ion was the base pKak using either LC/APCI-MS or LC/ISP-MS. Limits of detectio4 rangigg from 5 to 0.1 μg/L and 0.1−25 ng/L were found when 50−100 mL of river water was processed in full-scan and time-scheduled SIMsmodes, respectively. The proposed analytical met od was validated by participating in various interlaboratory exercisesedistributed by Aquachek (WRC, Medmenham, U.e.), using groundwa>er samples containing phenols at levels ranging from 0.1 to 2.5 μg/L.

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