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Headspace solid-phase microextraction of phthalic acid esters from vegetable oil employing solvent based matrix modification.
Anal Chim Acta. 2007 Jan 16; 582(1):24-33.AC

Abstract

A new solvent-free analytical procedure based on headspace solid-phase microextraction (SPME) coupled to gas chromatography employing an electron capture detector (GC/ECD) or alternatively a mass spectrometric detector (GC/MSD) has been developed for the determination of phthalic acid esters (dimethyl-[DMP], diethyl-[DEP], di-n-butyl-[DnBP], butylbenzyl-[BBP], di-2-ethylhexyl-[DEHP] and di-n-octyl [DnOP] phthalate) in vegetable oils. Four different fiber coatings were evaluated, among them polydimethylsiloxane with a thickness of 100 microm appeared to be the best choice for allowing extraction of the whole group of analytes. Various solvents were tested as sample matrix modification agents with the aim to facilitate the transfer of esters with low vapour pressure (DEHP and DnOP) from oil matrix into the headspace. The addition of methanol resulted in optimal set-up applicable for all phthalate esters. Temperature control and the way of sample stirring were recognized as critical points of the whole procedure. Primarily, because shaking rather than stirring of the sample is carried out using a CombiPal multipurpose sampler, the automation of the SPME method employing this instrument was found to be not fully suitable for efficient stripping of phthalates from the oil matrix into the sample headspace. Nevertheless, the optimized manual SPME method, encompassing GC/ECD or GC/MSD for the separation and detection of target analytes, offers a unique solution and showed acceptable performance characteristics: linear response in the range of 0.5-2 mg kg(-1) and repeatability expressed as R.S.D. between 14 and 23% at the spiking level of 2 mg kg(-1).

Authors+Show Affiliations

Institute of Chemical Technology, Department of Food Chemistry and Analysis, Technická 3, Prague 6, 166 28, Czech Republic. Katerina.Holadova@vscht.cz <Katerina.Holadova@vscht.cz>No 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

17386470

Citation

Holadová, Katerina, et al. "Headspace Solid-phase Microextraction of Phthalic Acid Esters From Vegetable Oil Employing Solvent Based Matrix Modification." Analytica Chimica Acta, vol. 582, no. 1, 2007, pp. 24-33.
Holadová K, Prokůpková G, Hajslová J, et al. Headspace solid-phase microextraction of phthalic acid esters from vegetable oil employing solvent based matrix modification. Anal Chim Acta. 2007;582(1):24-33.
Holadová, K., Prokůpková, G., Hajslová, J., & Poustka, J. (2007). Headspace solid-phase microextraction of phthalic acid esters from vegetable oil employing solvent based matrix modification. Analytica Chimica Acta, 582(1), 24-33.
Holadová K, et al. Headspace Solid-phase Microextraction of Phthalic Acid Esters From Vegetable Oil Employing Solvent Based Matrix Modification. Anal Chim Acta. 2007 Jan 16;582(1):24-33. PubMed PMID: 17386470.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Headspace solid-phase microextraction of phthalic acid esters from vegetable oil employing solvent based matrix modification. AU - Holadová,Katerina, AU - Prokůpková,Gabriela, AU - Hajslová,Jana, AU - Poustka,Jan, Y1 - 2006/09/08/ PY - 2006/06/07/received PY - 2006/09/02/revised PY - 2006/09/05/accepted PY - 2007/3/28/pubmed PY - 2007/6/1/medline PY - 2007/3/28/entrez SP - 24 EP - 33 JF - Analytica chimica acta JO - Anal Chim Acta VL - 582 IS - 1 N2 - A new solvent-free analytical procedure based on headspace solid-phase microextraction (SPME) coupled to gas chromatography employing an electron capture detector (GC/ECD) or alternatively a mass spectrometric detector (GC/MSD) has been developed for the determination of phthalic acid esters (dimethyl-[DMP], diethyl-[DEP], di-n-butyl-[DnBP], butylbenzyl-[BBP], di-2-ethylhexyl-[DEHP] and di-n-octyl [DnOP] phthalate) in vegetable oils. Four different fiber coatings were evaluated, among them polydimethylsiloxane with a thickness of 100 microm appeared to be the best choice for allowing extraction of the whole group of analytes. Various solvents were tested as sample matrix modification agents with the aim to facilitate the transfer of esters with low vapour pressure (DEHP and DnOP) from oil matrix into the headspace. The addition of methanol resulted in optimal set-up applicable for all phthalate esters. Temperature control and the way of sample stirring were recognized as critical points of the whole procedure. Primarily, because shaking rather than stirring of the sample is carried out using a CombiPal multipurpose sampler, the automation of the SPME method employing this instrument was found to be not fully suitable for efficient stripping of phthalates from the oil matrix into the sample headspace. Nevertheless, the optimized manual SPME method, encompassing GC/ECD or GC/MSD for the separation and detection of target analytes, offers a unique solution and showed acceptable performance characteristics: linear response in the range of 0.5-2 mg kg(-1) and repeatability expressed as R.S.D. between 14 and 23% at the spiking level of 2 mg kg(-1). SN - 1873-4324 UR - https://www.unboundmedicine.com/medline/citation/17386470/Headspace_solid_phase_microextraction_of_phthalic_acid_esters_from_vegetable_oil_employing_solvent_based_matrix_modification_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0003-2670(06)01846-0 DB - PRIME DP - Unbound Medicine ER -