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Determination of linear alkylbenzenesulfonates and their degradation products in solis by liquid chromatography-electrospray-ion trap multiple-stage mass spectrometry

AuthorsAndreu Pérez, V. ; Picó, Yolanda
KeywordsLinear alkylbenzenesulfonates
Sulfophenyl carboxylates
Electrospray-ion trap multiple-stage mass spectrometry
Sludge amendment
Analytical methodology
Fragmentation patterns
Issue Date15-May-2004
CitationAnalytical Chemistry 76(10): 2878-2885 (2004)
AbstractLinear alkylbenzenesulfonates (LAS) (C-10-C-13) and their degradation products, sulfophenyl carboxylate compounds (SPCs) (C-2-C-6, C-8, C-11), have been extracted from soil samples with methanol, isolated, concentrated by solid-phase extraction, and determined by liquid chromatography/negative ion electrospray quadrupole ion-trap tandem mass spectrometry (MSn). The ion fragmentation processes and pathways were studied in detail by MS, MS2, and MS3. Upon collision-induced dissociation, the deprotonated molecules of LASs render the ethylene-substituted benzenesulfonate ion (m/z 183), the fragmentation of which gave the intense signal at m/z 119, corresponding to the ethylene-substituted phenoxide ion formed by the loss of sulfur dioxide. The fragmentation pattern of SPCs shows that, for the analytes of large carbon atom chains (>5C), the neutral loss of water is favored whereas for those of short carbon atoms chain, the loss of carbon dioxide is more frequent. Multiple reaction monitoring using isolation only for MS and using isolation and fragmentation for MS2 and MS3 were used to identify and quantify each compound. The three MS modes have been validated in terms of sensitivity, selectivity, and precision, showing that each MS stage used reduces sensitivity 10 times. Recoveries from soil were higher than 65% at LOQ level for all the analytes tested, except for C-2-C-4 SPCs by any MS mode, with relative standard deviation lower than 19%. The utility of the method is demonstrated by successfully quantifying real samples treated with these products. Quantification limits for the methodology developed in this work ranged from 0.5 to 50 mug kg(-1) by MS, from 2 to 400 mug kg(-1) by MS2, and from 20 to 4000 mug kg(-1) by MS3. Concentration levels of LASs and SPCs-ranging from 0.1 to 15 mg kg(-1)-were found in soil samples amended with sludges, thus indicating their input and persistence in the soil compartment.
Description8 páginas, 3 figuras, 4 tablas.
Publisher version (URL)http://dx.doi.org//10.1021/ac035483e
Appears in Collections:(CIDE) Artículos
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