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Determination of synthetic phenolic antioxidants and their metabolites in water samples by downscaled solid-phase extraction, silylation and gas chromatography-mass spectrometry.
J Chromatogr A. 2010 Oct 08; 1217(41):6428-35.JC

Abstract

The development and performance evaluation of an analytical method dedicated to the comprehensive determination of the most relevant antioxidants and their metabolites in aqueous environmental samples is presented. This was achieved by a miniaturised solid-phase extraction (SPE) with 10mg Oasis HLB cartridges, which allow to achieve a concentration factor of 200, reducing organic solvent wastes (1 mL of ethyl acetate suffices for complete elution) and SPE costs and eliminating the need for solvent evaporation that otherwise compromises the recoveries of butylated hydroxytoluene (BHT) and 2,6-di-tert-butylcyclohexa-2,5-diene-1,4-dione (BHT-Q). Analytes were then determined by gas chromatography-mass spectrometry (GC-MS) after derivatisation with N-methyl-N-(tert-butyldimethylsilyl)-trifluoroacetamide (MTBSTFA) in a single run. BHT-d(7) and n-propyl-paraben-d(4) (PrP-d(4)) were used as surrogate internal standards. These surrogates allowed obtaining relative recoveries in the 80-110% range for all analytes even with complex wastewater samples and LODs at the 2-44 ngL(-1) level taking into account blank issues often associated to antioxidants analysis. The method was applied to sewage and river waters, showing that the seven analytes could be detected in raw wastewater. BHT and BHT-Q were the most concentrated species in that type of sample (in the 275-871 ngL(-1) range). On the other hand two metabolites of BHT, 3,5-di-tert-butyl-4-hydroxybenzaldehyde (BHT-CHO) and 3,5-di-tert-butyl-4-hydroxybenzoic acid (BHT-COOH) appeared to be the most ubiquitous species, being found in all samples in the 10-150 ngL(-1) concentration range.

Authors+Show Affiliations

Department of Analytical Chemistry, Nutrition and Food Sciences, IIAA - Institute for Food Analysis and Research, University of Santiago de Compostela, 15782 Santiago de Compostela, Spain.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

20817189

Citation

Rodil, Rosario, et al. "Determination of Synthetic Phenolic Antioxidants and Their Metabolites in Water Samples By Downscaled Solid-phase Extraction, Silylation and Gas Chromatography-mass Spectrometry." Journal of Chromatography. A, vol. 1217, no. 41, 2010, pp. 6428-35.
Rodil R, Quintana JB, Basaglia G, et al. Determination of synthetic phenolic antioxidants and their metabolites in water samples by downscaled solid-phase extraction, silylation and gas chromatography-mass spectrometry. J Chromatogr A. 2010;1217(41):6428-35.
Rodil, R., Quintana, J. B., Basaglia, G., Pietrogrande, M. C., & Cela, R. (2010). Determination of synthetic phenolic antioxidants and their metabolites in water samples by downscaled solid-phase extraction, silylation and gas chromatography-mass spectrometry. Journal of Chromatography. A, 1217(41), 6428-35. https://doi.org/10.1016/j.chroma.2010.08.020
Rodil R, et al. Determination of Synthetic Phenolic Antioxidants and Their Metabolites in Water Samples By Downscaled Solid-phase Extraction, Silylation and Gas Chromatography-mass Spectrometry. J Chromatogr A. 2010 Oct 8;1217(41):6428-35. PubMed PMID: 20817189.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Determination of synthetic phenolic antioxidants and their metabolites in water samples by downscaled solid-phase extraction, silylation and gas chromatography-mass spectrometry. AU - Rodil,Rosario, AU - Quintana,José Benito, AU - Basaglia,Giulia, AU - Pietrogrande,Maria Chiara, AU - Cela,Rafael, Y1 - 2010/08/13/ PY - 2010/06/18/received PY - 2010/07/29/revised PY - 2010/08/06/accepted PY - 2010/9/7/entrez PY - 2010/9/8/pubmed PY - 2010/12/21/medline SP - 6428 EP - 35 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1217 IS - 41 N2 - The development and performance evaluation of an analytical method dedicated to the comprehensive determination of the most relevant antioxidants and their metabolites in aqueous environmental samples is presented. This was achieved by a miniaturised solid-phase extraction (SPE) with 10mg Oasis HLB cartridges, which allow to achieve a concentration factor of 200, reducing organic solvent wastes (1 mL of ethyl acetate suffices for complete elution) and SPE costs and eliminating the need for solvent evaporation that otherwise compromises the recoveries of butylated hydroxytoluene (BHT) and 2,6-di-tert-butylcyclohexa-2,5-diene-1,4-dione (BHT-Q). Analytes were then determined by gas chromatography-mass spectrometry (GC-MS) after derivatisation with N-methyl-N-(tert-butyldimethylsilyl)-trifluoroacetamide (MTBSTFA) in a single run. BHT-d(7) and n-propyl-paraben-d(4) (PrP-d(4)) were used as surrogate internal standards. These surrogates allowed obtaining relative recoveries in the 80-110% range for all analytes even with complex wastewater samples and LODs at the 2-44 ngL(-1) level taking into account blank issues often associated to antioxidants analysis. The method was applied to sewage and river waters, showing that the seven analytes could be detected in raw wastewater. BHT and BHT-Q were the most concentrated species in that type of sample (in the 275-871 ngL(-1) range). On the other hand two metabolites of BHT, 3,5-di-tert-butyl-4-hydroxybenzaldehyde (BHT-CHO) and 3,5-di-tert-butyl-4-hydroxybenzoic acid (BHT-COOH) appeared to be the most ubiquitous species, being found in all samples in the 10-150 ngL(-1) concentration range. SN - 1873-3778 UR - https://www.unboundmedicine.com/medline/citation/20817189/Determination_of_synthetic_phenolic_antioxidants_and_their_metabolites_in_water_samples_by_downscaled_solid_phase_extraction_silylation_and_gas_chromatography_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(10)01072-1 DB - PRIME DP - Unbound Medicine ER -