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Use of headspace solid-phase microextraction coupled to liquid chromatography for the analysis of polycyclic aromatic hydrocarbons in tea infusions 2007 Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071, Murcia, Spain.
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Print(0)
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Journal Article
Periodical, Full
Journal of chromatography.A
Periodical, Abbrev.
J.Chromatogr.A
Pub Date Free Form
14-Sep
Volume
1164
Issue
2-Jan
Start Page
10
Other Pages
17
Notes
LR: 20090115; JID: 9318488; 0 (Polycyclic Hydrocarbons, Aromatic); 0 (Tea); 2007/04/02 [received]; 2007/06/20 [revised]; 2007/06/27 [accepted]; 2007/07/01 [aheadofprint]; ppublish
Place of Publication
Netherlands
ISSN/ISBN
0021-9673; 0021-9673
Accession Number
PMID: 17628570
Language
eng
SubFile
Journal Article; Research Support, Non-U.S. Gov't; IM
DOI
S0021-9673(07)01144-2 [pii]
Output Language
Unknown(0)
PMID
17628570
Abstract
A sensitive and solvent-free procedure for the determination of 11 polycyclic aromatic hydrocarbons in tea infusions using headspace solid-phase microextraction coupled to liquid chromatography with fluorimetric detection is described. A medium polarity polydimethylsiloxane-divinylbenzene 60 microm fiber was found to be suitable for extraction at 90 degrees C and with an extraction time of 60 min under continuous stirring. Desorption was carried out using the static mode for 5 min. Under the optimized conditions, when 1.75 g of tea sample were extracted with boiling water, the precision ranged from 4 to 16% (RSD) and detection limits were between 4 and 145 ngL(-1), depending on the compound. The reliability of the procedure was corroborated by means of GC-MS. The results obtained for a standard reference material were within the range indicated by the supplier.
Descriptors
Chromatography, Liquid/methods, Polycyclic Hydrocarbons, Aromatic/analysis/chemistry, Reproducibility of Results, Solid Phase Microextraction/methods, Tea/chemistry
Links
Book Title
Database
Publisher
Data Source
Authors
Vinas,P., Campillo,N., Aguinaga,N., Perez-Canovas,E., Hernandez-Cordoba,M.
Original/Translated Title
URL
Date of Electronic
20070701
PMCID
Editors
Headspace solid-phase microextraction-gas chromatography method for the determination of valproic acid in human serum, and formulations using hollow-fiber coated wire 2009 Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Iran. mafarajzadeh@yahoo.com
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Print(0)
Ref Type
Journal Article
Periodical, Full
Analytical sciences : the international journal of the Japan Society for Analytical Chemistry
Periodical, Abbrev.
Anal.Sci.
Pub Date Free Form
Jul
Volume
25
Issue
7
Start Page
875
Other Pages
879
Notes
LR: 20131121; JID: 8511078; 0 (Anticonvulsants); 0 (Pharmaceutical Preparations); 0 (Salts); 614OI1Z5WI (Valproic Acid); ppublish
Place of Publication
Japan
ISSN/ISBN
1348-2246; 0910-6340
Accession Number
PMID: 19609026
Language
eng
SubFile
Journal Article; IM
DOI
JST.JSTAGE/analsci/25.875 [pii]
Output Language
Unknown(0)
PMID
19609026
Abstract
A method was developed for the extraction of valproic acid (VPA) by hollow-fiber coated wire as a lab-made solid-phase microextraction (SPME) fiber and its determination by capillary gas chromatography in human serum and pharmaceutical formulations. In this study, a piece of copper wire coated by polypropylene hollow-fiber membrane was used as a SPME fiber, and its efficiency for the extraction of VPA from the headspace of samples prior to gas chromatographic analysis was evaluated. The optimum conditions of microextraction process were selected, and the limit of detection for VPA was found to be 85 microg L(-1) in solution and 1.7 mg L(-1) in human serum. A low detection limit, a wide linear dynamic range (0.25-100 mg L(-1)), good repeatability (RSD%<4 in formulations and RSD%<7 in serum samples) and a higher mechanical durability due to its metallic base are some of the most important advantages of the proposed fiber.
Descriptors
Anticonvulsants/blood/isolation & purification, Blood Chemical Analysis/methods, Chemistry, Pharmaceutical, Chromatography, Gas/methods, Humans, Hydrogen-Ion Concentration, Male, Pharmaceutical Preparations/chemistry, Reproducibility of Results, Salts/chemistry, Solid Phase Microextraction/instrumentation/methods, Solubility, Temperature, Time Factors, Valproic Acid/blood/isolation & purification
Links
Book Title
Database
Publisher
Data Source
Authors
Farajzadeh,M. A., Farhadi,K., Matin,A. A., Hashemi,P., Jouyban,A.
Original/Translated Title
URL
Date of Electronic
PMCID
Editors
Comparison of air-agitated liquid-liquid microextraction technique and conventional dispersive liquid-liquid micro-extraction for determination of triazole pesticides in aqueous samples by gas chromatography with flame ionization detection 2013 Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran. mafarajzadeh@yahoo.com
Source Type
Print(0)
Ref Type
Journal Article
Periodical, Full
Journal of chromatography.A
Periodical, Abbrev.
J.Chromatogr.A
Pub Date Free Form
26-Jul
Volume
1300
Issue
Start Page
70
Other Pages
78
Notes
LR: 20151119; CI: Copyright (c) 2013; JID: 9318488; 0 (Pesticide Residues); 0 (Triazoles); 1N41638RNO (Ethylene Dibromide); 451W47IQ8X (Sodium Chloride); Y4S76JWI15 (Methanol); OTO: NOTNLM; 2012/11/28 [received]; 2013/02/11 [revised]; 2013/02/12 [accepted
Place of Publication
Netherlands
ISSN/ISBN
1873-3778; 0021-9673
Accession Number
PMID: 23473511
Language
eng
SubFile
Journal Article; Research Support, Non-U.S. Gov't; IM
DOI
10.1016/j.chroma.2013.02.033 [doi]
Output Language
Unknown(0)
PMID
23473511
Abstract
Two micro-extraction methods, air-agitated liquid-liquid microextraction (AALLME) and dispersive liquid-liquid microextraction (DLLME), have been compared with each other by applying them for the analysis of five triazole pesticides (penconazole, hexaconazole, diniconazole, tebuconazole and triticonazole) in aqueous samples by gas chromatography with flame ionization detection (GC-FID). In the AALLME method, which excludes any disperser solvent, much less volume of organic solvent is used. In order to form fine and dispersed organic droplets in the aqueous phase, the mixture of aqueous sample solution and extraction solvent is repeatedly aspirated and dispensed with a syringe. In the DLLME method, an appropriate mixture of extraction solvent and disperser solvent is rapidly injected by a syringe into the aqueous sample. Effect of the pertinent experimental factors on DLLME (i.e. identity and volume of the extraction and disperser solvents and ionic strength) and on AALLME (identity and volume of the extraction solvent, number of agitations, and ionic strength) were investigated. Under optimal conditions, limits of detection for the five target pesticides obtained by AALLME-GC-FID and DLLME-GC-FID ranged from 0.20 to 1.1ngmL(-1) and 1.9 to 5.9ngmL(-1), respectively. The relative standard deviations (RSDs, n=5) were in the range of 1-4% and 3-5% with the enrichment factors of 449-504 and 79-143 for AALLME-GC-FID and DLLME-GC-FID, respectively. Both of the compared methods are simple, fast, efficient, inexpensive and can be applied to the analysis of the five pesticides in different aqueous samples in which penconazole and hexaconazole were found. For spiked samples, the recoveries were in the ranges of 92-105%, and 92-104% for AALLME and DLLME, respectively.
Descriptors
Links
Book Title
Database
Publisher
Elsevier B.V
Data Source
Authors
Farajzadeh,M.A., Mogaddam,M.R., Aghdam,A.A.
Original/Translated Title
URL
Date of Electronic
20130219
PMCID
Editors
Quantitative detection of bisphenol A and bisphenol A diglycidyl ether metabolites in human plasma by liquid chromatography-electrospray mass spectrometry 2001 Department of Analytical Chemistry, Faculty of Pharmaceutical Sciences, Hoshi University, Tokyo, Japan.
Source Type
Print(0)
Ref Type
Journal Article
Periodical, Full
Journal of chromatography.B, Biomedical sciences and applications
Periodical, Abbrev.
J.Chromatogr.B Biomed.Sci.Appl.
Pub Date Free Form
25-Dec
Volume
765
Issue
2
Start Page
121
Other Pages
126
Notes
LR: 20131121; JID: 9714109; 0 (Benzhydryl Compounds); 0 (Epoxy Compounds); 0 (Phenols); F3XRM1NX4H (2,2-bis(4-glycidyloxyphenyl)propane); MLT3645I99 (bisphenol A); ppublish
Place of Publication
Netherlands
ISSN/ISBN
1387-2273; 1387-2273
Accession Number
PMID: 11767304
Language
eng
SubFile
Journal Article; Research Support, Non-U.S. Gov't; IM
DOI
Output Language
Unknown(0)
PMID
11767304
Abstract
Due to the ubiquity of epoxy resin compounds and their potential role in increasing the risk for reproductive dysfunction and cancer, the need for an assessment of human exposure is urgent. Therefore, we developed a method for measuring bisphenol A (BPA) and bisphenol A diglycidyl ether (BADGE) metabolites in human blood samples using high-performance liquid chromatography-electrospray ionization mass spectrometry (LC-MS). Human blood samples were processed using enzymatic deconjugation of the glucuronides followed by a novel sample preparation procedure using a solid-phase-cartridge column. This selective analytical method permits rapid detection of the metabolites, free BPA and a hydrolysis product of BADGE (BADGE-40H) with detection limits in the low nanogram per milliliter range (0.1 ng ml(-1) of BPA and 0.5 ng ml(-1) of BADGE-40H). The sample extraction was achieved by Oasis HLB column on gradient elution. The recoveries of BPA and BADGE-40H added to human plasma samples were above 70.0% with a standard deviation of less than 5.0%. This selective, sensitive and accurate method will assist in elucidating potential associations between human exposure to epoxy-based compounds and adverse health effects.
Descriptors
Benzhydryl Compounds, Chromatography, Liquid/methods, Epoxy Compounds/analysis, Humans, Phenols/blood, Spectrometry, Mass, Electrospray Ionization/methods
Links
Book Title
Database
Publisher
Data Source
Authors
Inoue,K., Yamaguchi,A., Wada,M., Yoshimura,Y., Makino,T., Nakazaw,H.
Original/Translated Title
URL
Date of Electronic
PMCID
Editors
Solid-phase extraction combined with large volume injection-programmable temperature vaporization-gas chromatography-mass spectrometry for the multiresidue determination of priority and emerging organic pollutants in wastewater 2012 Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country-UPV/EHU, PK 644, 48080 Bilbao, Spain.
Source Type
Print(0)
Ref Type
Journal Article
Periodical, Full
Journal of chromatography.A
Periodical, Abbrev.
J.Chromatogr.A
Pub Date Free Form
20-Jul
Volume
1247
Issue
Start Page
104
Other Pages
117
Notes
CI: Copyright (c) 2012; JID: 9318488; 0 (Organic Chemicals); 0 (Water Pollutants, Chemical); 2012/02/27 [received]; 2012/04/16 [revised]; 2012/05/06 [accepted]; 2012/05/14 [aheadofprint]; ppublish
Place of Publication
Netherlands
ISSN/ISBN
1873-3778; 0021-9673
Accession Number
PMID: 22673809
Language
eng
SubFile
Journal Article; Research Support, Non-U.S. Gov't; IM
DOI
10.1016/j.chroma.2012.05.022 [doi]
Output Language
Unknown(0)
PMID
22673809
Abstract
In the present work the simultaneous extraction for the multiresidue determination in wastewater samples of organic compounds such as polychlorinated biphenyls (PCBs), polybrominated biphenyls (PBBs), pesticides, polycyclic aromatic hydrocarbons (PAHs), phthalate esters (PEs), alkylphenols (APs), bisphenol A (BPA) or hormones included in different lists of priority and emerging pollutants because of their action as endocrine disrupting compounds (EDCs) was developed. Different solid phase extraction (SPE) variables such as the nature of the solid phase (Oasis-HLC, C18 and Lichrolut), the sample volume, the addition of MeOH and NaCl, the pH of the water phase and the volume of the eluent solvent were optimized in order to analyze simultaneously the priority and emerging families of pollutants mentioned above. Good recoveries were obtained for Milli-Q water (80-120%), however, since the use of deuterated analogues and dilution of the sample did not correct the matrix effect, additional SPE clean-up step using Florisil(R) cartridges was necessary to obtain good results for wastewater samples (80-125%). In order to improve the limits of detection (LODs), large volume injection (LVI) using programmable temperature vaporizer (PTV) coupled to gas chromatography-mass spectrometry (GC-MS) was also optimized. Since analytes losses in the case of the most volatile congeners occurred during the derivatization step and no separation of the derivatized and the non-derivatized analytes was possible during SPE elution, two different injections were optimized for each analyte group. LODs were in good agreement with those found in the literature and relative standard deviations (RSDs) were in the 10-25% range for Milli-Q and 12-30% for wastewater samples. The method was finally applied to the determination of target analytes in three different wastewater treatment plants (WWTPs, Bakio, Gernika and Galindo (Spain)) and in one water purification plant (WPP) in Zornotza (Spain).
Descriptors
Links
Book Title
Database
Publisher
Elsevier B.V
Data Source
Authors
Bizkarguenaga,E., Ros,O., Iparraguirre,A., Navarro,P., Vallejo,A., Usobiaga,A., Zuloaga,O.
Original/Translated Title
URL
Date of Electronic
20120514
PMCID
Editors
Determination of organic priority pollutants and emerging compounds in wastewater and snow samples using multiresidue protocols on the basis of microextraction by packed sorbents coupled to large volume injection gas chromatography-mass spectrometry analy 2010 Department of Analytical Chemistry, Helmholtz Centre for Environmental Research-UFZ Permoserstrasse 15, D-04318 Leipzig, Germany. ailette.prieto-sobrina@ufz.de
Source Type
Print(0)
Ref Type
Journal Article
Periodical, Full
Journal of chromatography.A
Periodical, Abbrev.
J.Chromatogr.A
Pub Date Free Form
17-Sep
Volume
1217
Issue
38
Start Page
6002
Other Pages
6011
Notes
LR: 20131121; CI: 2010; JID: 9318488; 0 (Humic Substances); 0 (Phenols); 0 (Phthalic Acids); 0 (Polycyclic Hydrocarbons, Aromatic); 0 (Sewage); 0 (Water Pollutants, Chemical); DFC2HB4I0K (Polychlorinated Biphenyls); 2010/05/21 [received]; 2010/07/22 [revi
Place of Publication
Netherlands
ISSN/ISBN
1873-3778; 0021-9673
Accession Number
PMID: 20719318
Language
eng
SubFile
Journal Article; IM
DOI
10.1016/j.chroma.2010.07.070 [doi]
Output Language
Unknown(0)
PMID
20719318
Abstract
This paper describes the development and validation of a new procedure for the simultaneous determination of 41 multi-class priority and emerging organic pollutants in water samples using microextraction by packed sorbent (MEPS) followed by large volume injection-gas chromatography-mass spectrometry (LVI-GC-MS). Apart from method parameter optimization the influence of humic acids as matrix components on the extraction efficiency of MEPS procedure was also evaluated. The list of target compounds includes polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), phthalate esters (PEs), nonylphenols (NPs), bisphenol A (BPA) and selected steroid hormones. The performance of the new at-line microextraction-LVI-GC-MS protocol was compared to standard solid-phase extraction (SPE) and LVI-GC-MS analysis. LODs for 100 mL samples (SPE) ranged from 0.2 to 736 ng L(-1) were obtained. LODs for 800 microL of sample (MEPS) were between 0.2 and 266 ng L(-1). In the case of MEPS methodology even a sample volume of only 800 microL allowed to detect the target compounds. These results demonstrate the high sensitivity of both procedures which permitted to obtain good recoveries (>75%) for all cases. The precision of the methods, calculated as relative standard deviation (RSD) was below 21% for all compounds and both methodologies. Finally, the developed methods were applied to the determination of target analytes in various samples, including snow and wastewater.
Descriptors
Gas Chromatography-Mass Spectrometry/methods, Humic Substances, Phenols/analysis/chemistry, Phthalic Acids/analysis/chemistry, Polychlorinated Biphenyls/analysis/chemistry, Polycyclic Hydrocarbons, Aromatic/analysis/chemistry, Reproducibility of Results, Sewage/chemistry, Snow/chemistry, Solid Phase Microextraction/methods, Water Pollutants, Chemical/analysis/chemistry
Links
Book Title
Database
Publisher
Elsevier B.V
Data Source
Authors
Prieto,A., Schrader,S., Moeder,M.
Original/Translated Title
URL
Date of Electronic
20100803
PMCID
Editors
Ionic liquid coated magnetic nanoparticles for the gas chromatography/mass spectrometric determination of polycyclic aromatic hydrocarbons in waters 2013 Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building, Campus de Rabanales, University of Cordoba, 14071 Cordoba, Spain.
Source Type
Print(0)
Ref Type
Journal Article
Periodical, Full
Journal of chromatography.A
Periodical, Abbrev.
J.Chromatogr.A
Pub Date Free Form
26-Jul
Volume
1300
Issue
Start Page
134
Other Pages
140
Notes
CI: Copyright (c) 2013; JID: 9318488; 0 (Drinking Water); 0 (Imidazoles); 0 (Ionic Liquids); 0 (Magnetite Nanoparticles); 0 (Polycyclic Hydrocarbons, Aromatic); 0 (Water Pollutants, Chemical); OTO: NOTNLM; 2012/12/11 [received]; 2013/03/07 [revised]; 2013
Place of Publication
Netherlands
ISSN/ISBN
1873-3778; 0021-9673
Accession Number
PMID: 23601292
Language
eng
SubFile
Journal Article; Research Support, Non-U.S. Gov't; IM
DOI
10.1016/j.chroma.2013.03.026 [doi]
Output Language
Unknown(0)
PMID
23601292
Abstract
In this paper, ionic liquid coated magnetic nanoparticles (IL-MNPs) have been prepared by covalent immobilization. The as-synthesized MNPs have been successfully used as sorbent for the extraction of polycyclic aromatic hydrocarbons (PAHs) from water samples, the analytes being finally determined by gas chromatography/mass spectrometry. The influence of several experimental variables (including the ionic strength, amount of MNPs, sample volume, agitation time and desorption solvent) has been considered in depth in the optimization process. The developed method, which has been analytically characterized under its optimal operation conditions, allows the detection of the analytes in the samples with method detection limits in the range from 0.04mugL(-1) (fluoranthene) to 1.11mugL(-1) (indeno(1,2,3-cd)pyrene). The repeatability of the method, expressed as relative standard deviation (RSD, n=7), varies between 4.0% (benzo[b]fluoranthene) and 8.9% (acenaphthene), while the enrichment factors are in the range from 49 (naphthalene) to 158 (fluoranthene). The proposed procedure has been applied for the determination of thirteen PAHs in water samples (tap, river, well and reservoir ones) with recoveries in the range from 75 to 102%.
Descriptors
Links
Book Title
Database
Publisher
Elsevier B.V
Data Source
Authors
Galan-Cano,F., Alcudia-Leon Mdel,C., Lucena,R., Cardenas,S., Valcarcel,M.
Original/Translated Title
URL
Date of Electronic
20130402
PMCID
Editors
Temporal distribution, behaviour and reactivities of BTEX compounds in a suburban Atlantic area during a year 2009 Department of Analytical Chemistry, University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna, Spain.
Source Type
Print(0)
Ref Type
Journal Article
Periodical, Full
Journal of environmental monitoring : JEM
Periodical, Abbrev.
J.Environ.Monit.
Pub Date Free Form
Jun
Volume
11
Issue
6
Start Page
1216
Other Pages
1225
Notes
LR: 20131121; JID: 100968688; 0 (Air Pollutants); 0 (Benzene Derivatives); 0 (Vehicle Emissions); 0 (Xylenes); 3FPU23BG52 (Toluene); J64922108F (Benzene); L5I45M5G0O (ethylbenzene); 2009/04/02 [aheadofprint]; 2009/06/01 [epublish]; ppublish
Place of Publication
England
ISSN/ISBN
1464-0333; 1464-0325
Accession Number
PMID: 19513453
Language
eng
SubFile
Journal Article; Research Support, Non-U.S. Gov't; IM
DOI
10.1039/b819370c [doi]
Output Language
Unknown(0)
PMID
19513453
Abstract
The temporal distribution of BTEX compounds (benzene, toluene, ethylbenzene and xylene isomers) in ambient air was studied in a suburban Atlantic area in the northwest of Spain. These compounds mean serious risks for public and occupational health and for biological and physical environments. A total of 1200 samples were analysed during a year, and in most of the samples toluene was the most abundant VOC followed by benzene or m+p-xylene. The average concentrations were 1.62, 2.15, 0.60, 0.94 and 0.47 microg m(-3) for benzene, toluene, ethylbenzene, m+p-xylenes and o-xylene respectively, although they reached values as high as 50.53, 28.57, 21.33, 46.13 and 22.74 microg m(-3) for the compounds in the same order. An exhaustive study was carried out to establish how both emission sources and the climatic conditions affected the BTEX levels measured in the outskirts of a small city. Wind directions and speeds, daily and seasonal BTEX profiles, ratios among the concentrations measured in the sampling site, in the city centre and in the fuels commonly used by the cars in the city were studied. The pollution roses revealed the presence of diffuse BTEX sources affecting the sampling point, although all the compounds reached their highest levels when the wind blew from an industrial area in the SW of the city. The daily BTEX profiles were well-correlated with the traffic pattern in the accesses to the city and the seasonal profile showed that the highest concentrations were reported in summertime. The ratios T/B, m+p-X/B and o-X/B were 1.32, 0.58 and 0.29 respectively; these values were lower than the ones reported in previous studies carried out in the centre of the same city. This could be caused by the major distance from the sampling point to the city centre and by the changes in the fuels and in the kind of vehicles used in the city. The correlation coefficients among the TEX fraction were always higher than 0.72 but benzene only showed a good correlation with these compounds in winter. The correlations between BTEX concentrations and their contributions to the photochemistry in the sampling area were used in order to evaluate the distance from the road traffic source and to estimate the presence of fresh or old air masses in the sampling point. This study provides data which can be useful to establish the BTEX levels in suburban areas from the coastal Atlantic region and improves the knowledge of the BTEX presence in this kind of area.
Descriptors
Air Pollutants/analysis, Atmosphere, Benzene/analysis, Benzene Derivatives/analysis, Cities, Environmental Monitoring, Humans, Seasons, Spain, Suburban Health, Temperature, Toluene/analysis, Vehicle Emissions/analysis, Volatilization, Wind, Xylenes/analysis
Links
Book Title
Database
Publisher
Data Source
Authors
Perez-Rial,D., Lopez-Mahia,P., Muniategui-Lorenzo,S., Prada-Rodriguez,D.
Original/Translated Title
URL
Date of Electronic
20090402
PMCID
Editors
Pressurized hot water extraction coupled to solid-phase microextraction-gas chromatography-mass spectrometry for the analysis of polycyclic aromatic hydrocarbons in sediments 2008 Department of Analytical Chemistry, University of A Coruna, Campus da Zapateira, A Coruna, Spain.
Source Type
Print(0)
Ref Type
Journal Article
Periodical, Full
Journal of chromatography.A
Periodical, Abbrev.
J.Chromatogr.A
Pub Date Free Form
4-Jul
Volume
1196-1197
Issue
Start Page
65
Other Pages
72
Notes
LR: 20090115; JID: 9318488; 0 (Polycyclic Hydrocarbons, Aromatic); 0 (Water Pollutants, Chemical); 2008/03/07 [received]; 2008/04/30 [revised]; 2008/05/07 [accepted]; 2008/05/10 [aheadofprint]; ppublish
Place of Publication
Netherlands
ISSN/ISBN
0021-9673; 0021-9673
Accession Number
PMID: 18501367
Language
eng
SubFile
Journal Article; Research Support, Non-U.S. Gov't; IM
DOI
10.1016/j.chroma.2008.05.006 [doi]
Output Language
Unknown(0)
PMID
18501367
Abstract
A fully automated, environmentally friendly, simple, and sensitive method was developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) in sediment samples. The procedure is based on pressurized hot water extraction (PHWE) followed by solid-phase microextraction (SPME) and determination by gas chromatography-mass spectrometry. For PHWE, parameters such as organic modifier, percentage of organic modifier, temperature, and static extraction time were studied. For SPME, extraction temperature and time, desorption temperature and time, splitless time, ionic strength adjustments, and effect of an organic modifier were studied. When these parameters were selected, the figures of merit were calculated. The detection and quantification limits were between 0.4-15 microg kg(-1) and 1.2-51 microg kg(-1), respectively. The linearity of the method was assessed spiking sediment samples at seven levels of concentration ranged between 2.5 microg kg(-1) and 500 microg kg(-1) for most of the studied PAHs. The method was validated by two concentration levels reference marine sediment materials (SRM 1944 and SRM 1941b). The obtained results are in very good agreement with the certificate materials. The developed method seems to be suitable for the analysis of PAHs at ultratrace levels in environmental matrices as sediment samples.
Descriptors
Chemical Fractionation/instrumentation/methods, Gas Chromatography-Mass Spectrometry/instrumentation/methods, Geologic Sediments/analysis/chemistry, Polycyclic Hydrocarbons, Aromatic/analysis/chemistry, Reproducibility of Results, Solid Phase Microextraction/instrumentation/methods, Water Pollutants, Chemical/analysis/isolation & purification
Links
Book Title
Database
Publisher
Data Source
Authors
Fernandez-Gonzalez,V., Concha-Grana,E., Muniategui-Lorenzo,S., Lopez-Mahia,P., Prada-Rodriguez,D.
Original/Translated Title
URL
Date of Electronic
20080510
PMCID
Editors
Solid-phase microextraction-gas chromatographic-tandem mass spectrometric analysis of polycyclic aromatic hydrocarbons. Towards the European Union water directive 2006/0129 EC 2007 Department of Analytical Chemistry, University of A Coruna, Campus da Zapateira, E-15071 A Coruna, Spain.
Source Type
Print(0)
Ref Type
Journal Article
Periodical, Full
Journal of chromatography.A
Periodical, Abbrev.
J.Chromatogr.A
Pub Date Free Form
28-Dec
Volume
1176
Issue
2-Jan
Start Page
48
Other Pages
56
Notes
LR: 20090115; JID: 9318488; 0 (Polycyclic Compounds); 0 (Water Pollutants, Chemical); 2007/08/16 [received]; 2007/10/31 [revised]; 2007/11/02 [accepted]; 2007/11/09 [aheadofprint]; ppublish
Place of Publication
Netherlands
ISSN/ISBN
0021-9673; 0021-9673
Accession Number
PMID: 18037429
Language
eng
SubFile
Journal Article; Research Support, Non-U.S. Gov't; IM
DOI
S0021-9673(07)01924-3 [pii]
Output Language
Unknown(0)
PMID
18037429
Abstract
This article presents a solid-phase microextraction (SPME) procedure to determine 27 parent and alkylated polycyclic aromatic hydrocarbons (PAHs) with diverging polarities and molecular masses in various types of water samples (tap, well, superficial, and seawater). A 65-microm polydimethylsiloxane-divinylbenzene (PDMS/DVB) fiber was used, and parameters affecting the extraction procedures such as extraction temperature and time, desorption temperature and time, splitless time, effect of an organic modifier or ionic adjustment were studied. The linearity and precision of the proposed method were satisfactory. The use of GC-MS determination in the full scan mode, in the selected ion monitoring (SIM) mode, and in the GC-MS-MS mode provided the unequivocal identification and quantification of the target analytes. Moreover, the proposed SPME-GC-MS-MS method, extracting only 18 ml of sample, reached the very restrictive limits fixed by the 2006/0129 EC proposal for a new water directive to be achieved by 2015. The matrix effects were evaluated through the analysis of tap, well, superficial, and seawater. A discussion on different behaviors, a result of the matrix effects, was included. Analytical recoveries were satisfactory in all cases. The novelty of this work consisted in the wide range of analyzed PAHs, the very low detection limits that were reached, the coupling of SPME-GC-MS-MS, and the study of the matrix effect on water samples. With this developed procedure, detection limits between 0.07 and 0.76 ng l(-1) and quantification limits between 0.10 and 0.98 ng l(-1) were obtained with MS-MS detection. Moreover, the analytical recoveries for different aqueous matrices were near 100% in all cases.
Descriptors
European Union, Gas Chromatography-Mass Spectrometry/methods, Hydrogen-Ion Concentration, Osmolar Concentration, Polycyclic Compounds/analysis, Tandem Mass Spectrometry/methods, Water Pollutants, Chemical/analysis
Links
Book Title
Database
Publisher
Data Source
Authors
Fernandez-Gonzalez,V., Concha-Grana,E., Muniategui-Lorenzo,S., Lopez-Mahia,P., Prada-Rodriguez,D.
Original/Translated Title
URL
Date of Electronic
20071109
PMCID
Editors