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A novel solid-phase microextraction using coated fiber based sol-gel technique using poly(ethylene glycol) grafted multi-walled carbon nanotubes for determination of benzene, toluene, ethylbenzene and o-xylene in water samples with gas chromatography-flam 2011 Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, Iran. asyazdi@um.ac.ir
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Print(0)
Ref Type
Journal Article
Periodical, Full
Journal of chromatography.A
Periodical, Abbrev.
J.Chromatogr.A
Pub Date Free Form
26-Aug
Volume
1218
Issue
34
Start Page
5757
Other Pages
5764
Notes
LR: 20151119; CI: Copyright (c) 2011; JID: 9318488; 0 (Benzene Derivatives); 0 (Nanotubes, Carbon); 0 (Water Pollutants, Chemical); 0 (Xylenes); 30IQX730WE (Polyethylene Glycols); 3FPU23BG52 (Toluene); J64922108F (Benzene); L5I45M5G0O (ethylbenzene); Z247
Place of Publication
Netherlands
ISSN/ISBN
1873-3778; 0021-9673
Accession Number
PMID: 21782185
Language
eng
SubFile
Evaluation Studies; Journal Article; Research Support, Non-U.S. Gov't; IM
DOI
10.1016/j.chroma.2011.06.099 [doi]
Output Language
Unknown(0)
PMID
21782185
Abstract
In this study, poly(ethylene glycol) (PEG) grafted onto multi-walled carbon nanotubes (PEG-g-MWCNTs) were synthesized by the covalent functionalization of MWCNTs with hydroxyl-terminated PEG chains. For the first time, functionalized product of PEG-g-MWCNTs was used as selective stationary phase to prepare the sol-gel solid-phase microextraction (SPME) fiber in combination with gas chromatography-flame ionization detector (GC-FID) for the determination of ultra-trace levels of benzene, toluene, ethylbenzene and o-xylene (BTEX) in real water samples. The PEG-g-MWCNTs were characterized by Fourier transform infrared spectra and also thermo-gravimetric analysis, which verified that PEG chains were grafted onto the surface of the MWCNTs. The scanning electron micrographs of the fiber surface revealed a highly porous structure which greatly increases the surface area for PEG-g-MWCNTs sol-gel coating. This fiber demonstrated many inherent advantages, the main being the strong anchoring of the coating to the fused silica resulting from chemical bonding with the silanol groups on the fused-silica fiber surface. The new PEG-g-MWCNTs sol-gel fiber is simple to prepare, robust, with high thermal stability and long lifetime, up to 200 extractions. Important parameters influencing the extraction efficiency such as desorption temperature and time, extraction temperature, extraction time, stirring speed and salt effect were investigated and optimized. Under the optimal conditions, the method detection limits (S/N=3) were in the range of 0.6-3 pg mL(-1) and the limits of quantification (S/N=10) between 2 and 10 pg mL(-1). The relative standard deviations (RSDs) for one fiber (repeatability) (n=5) were obtained from 4.40 up to 5.75% and between fibers or batch to batch (n=3) (reproducibility) in the range of 4.31-6.55%. The developed method was successfully applied to real water samples while the relative recovery percentages obtained for the spiked water samples at 20 pg mL(-1) were from 90.21 to 101.90%.
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Book Title
Database
Publisher
Elsevier B.V
Data Source
Authors
Sarafraz-Yazdi,A., Amiri,A., Rounaghi,G., Hosseini,H.E.
Original/Translated Title
URL
Date of Electronic
20110703
PMCID
Editors
Optimization of a GC/MS procedure that uses parallel factor analysis for the determination of bisphenols and their diglycidyl ethers after migration from polycarbonate tableware 2013 Department of Chemistry, Faculty of Sciences, University of Burgos, Plaza Misael Banuelos s/n, 09001 Burgos, Spain.
Source Type
Print(0)
Ref Type
Journal Article
Periodical, Full
Talanta
Periodical, Abbrev.
Talanta
Pub Date Free Form
15-Mar
Volume
106
Issue
Start Page
266
Other Pages
280
Notes
CI: Copyright (c) 2012; JID: 2984816R; 0 (Benzhydryl Compounds); 0 (Epoxy Compounds); 0 (Epoxy Resins); 0 (Phenols); 0 (Polycarboxylate Cement); 0 (bisphenol F diglycidyl ether); 25766-59-0 (polycarbonate); MLT3645I99 (bisphenol A); QD2C19044Z (4,4'-bisph
Place of Publication
Netherlands
ISSN/ISBN
1873-3573; 0039-9140
Accession Number
PMID: 23598127
Language
eng
SubFile
Journal Article; Research Support, Non-U.S. Gov't; IM
DOI
10.1016/j.talanta.2012.10.086 [doi]
Output Language
Unknown(0)
PMID
23598127
Abstract
Bisphenol A (BPA), bisphenol F (BPF) and their corresponding diglycidyl ethers (BADGE and BFDGE) are simultaneously determined using a programmed-temperature vaporizer-gas chromatography/mass spectrometry (PTV-GC/MS) system. BPA is used in the production of polycarbonate (PC), whereas BADGE and BFDGE are for manufacturing epoxy resins. Several food alerts caused by the migration of this kind of substances from contact food materials have led to the harmonization of the European legislation in Commission Regulation (EU) No. 10/2011, in force from 14 January 2011. In consequence, the use of BPA has been prohibited in the manufacture of plastic infant feeding bottles from 1 May 2011 and from 1 June 2011 regarding the placing on the market and importation into the European Union. Recently, the French Parliament has decreed that the presence of BPA in any food containers will be banned. Similarly, the use and/or presence of BFDGE are not allowed. In this work, a GC/MS method has been developed for the simultaneous determination of BPF, BPA, BFDGE and BADGE. For each one of the I samples that are analyzed, the abundance of J characteristic m/z ratios is recorded at K times around the retention time of each peak, so a data tensor of dimension IxJxK is obtained for every analyte. The decomposition of this tensor by means of parallel factor analysis (PARAFAC) enables to: (a) identify unequivocally each analyte according to the maximum permitted tolerances for relative ion intensities, and (b) quantify each analyte, even in the presence of coeluents. This identification, based on the mass spectrum and the retention time, guarantees the specificity of the analysis. This specificity could fail if the total ion chromatogram (TIC) is considered when there is poor resolution between some peaks or whether interferents coelute. With the aim of studying the effect of shortening the time of the analysis on the quality of the determinations while maintaining the specificity of the identifications, two of the heating ramps in the oven temperature program are changed according to a two-level factorial design. Each analyte is identified by means of a PARAFAC decomposition of a data tensor obtained from several concentration levels, in such a way that five figures of merit are calculated for each experiment of the design. The analysis of these figures of merit for the 16 objects (4 compoundsx4 heating ramps) using principal component analysis (PCA) shows that the shortest temperature program should be considered, since this is the one the best figures of merit for BPA and BFDGE (both banned) are achieved with. At these conditions and with probabilities of false positive and false negative fixed at 0.05, values of detection capability (CCbeta) between 2.65 and 4.71 mug L(-1) when acetonitrile is the injection solvent, and between 1.97 and 5.53 mug L(-1) when acetone, are obtained. This GC/MS method has been applied to the simultaneous determination of BPF, BPA, BFDGE and BADGE in food simulant D1 (ethanol-H2O, 1:1 v/v), which had been previously in contact with PC tableware for 24h at 70 degrees C and then pretreated by a solid-phase extraction (SPE) step. The migration of BPA from the new PC containers analyzed is confirmed, and values between 104.67 and 181.46 mug L(-1) (0.73 and 1.27 mug L(-1) after correction) of BPA have been estimated. None of the results obtained exceeds the specific migration limit of 600 mug L(-1) established by law for BPA in plastic food materials different from PC infant feeding bottles. Severe problems of coelution of interferents have been overcome using PARAFAC decompositions in the analysis of these food simulant samples.
Descriptors
Links
Book Title
Database
Publisher
Elsevier B.V
Data Source
Authors
Oca,M.L., Ortiz,M.C., Herrero,A., Sarabia,L.A.
Original/Translated Title
URL
Date of Electronic
20121102
PMCID
Editors
Optimum pH for the determination of bisphenols and their corresponding diglycidyl ethers by gas chromatography-mass spectrometry. Migration kinetics of bisphenol A from polycarbonate glasses 2014 Department of Chemistry, Faculty of Sciences, University of Burgos, Plaza Misael Banuelos s/n, 09001 Burgos, Spain.; Department of Mathematics and Computation, Faculty of Sciences, University of Burgos, Plaza Misael Banuelos s/n, 09001 Burgos, Spain.; Dep
Source Type
Print(0)
Ref Type
Journal Article
Periodical, Full
Journal of chromatography.A
Periodical, Abbrev.
J.Chromatogr.A
Pub Date Free Form
19-Sep
Volume
1360
Issue
Start Page
23
Other Pages
38
Notes
CI: Copyright (c) 2014; JID: 9318488; 0 (Benzhydryl Compounds); 0 (Ethers); 0 (Phenols); 0 (Polycarboxylate Cement); 0 (Polymers); 25766-59-0 (polycarbonate); MLT3645I99 (bisphenol A); OTO: NOTNLM; 2014/06/11 [received]; 2014/07/18 [revised]; 2014/07/21 [
Place of Publication
Netherlands
ISSN/ISBN
1873-3778; 0021-9673
Accession Number
PMID: 25113873
Language
eng
SubFile
Journal Article; Research Support, Non-U.S. Gov't; IM
DOI
10.1016/j.chroma.2014.07.063 [doi]
Output Language
Unknown(0)
PMID
25113873
Abstract
This paper presents, on the one hand, the study of the influence of the pH of the medium on the determination of bisphenol F (BPF), bisphenol A (BPA) and their corresponding diglycidyl ethers (BFDGE and BADGE, respectively) by GC-MS after a solid-phase extraction step, using BPA-d16 as internal standard and Parallel Factor Analysis (PARAFAC) decomposition as a multi-way tool for the unequivocal identification and quantification of the four analytes. As the structure of both BFDGE and BADGE has two 2,3-epoxypropoxy groups that can undergo an acid- or base-catalyzed ring-opening via nucleophilic substitution reactions, several samples spiked with the four analytes were set to different pH values between 2 and 12. The best results were obtained in the pH region 8-10, being 9 the most suitable value. Coelution of interferents was overcome using the PARAFAC decomposition; otherwise, the presence of some analytes could not have been ensured according to the regulations currently in force. Secondly, the release of BPA from polycarbonate glasses into food simulant D1 (ethanol 50% (v/v)) over time was studied through seven migration tests and the differences found in this migration process with the incubation temperature (50 and 70 degrees C) were evaluated. A nonlinear regression was used to fit the experimental data following an exponential relation between the concentration of BPA transferred from every glass and the respective migration test. None of the quantities of BPA released exceeded the specific migration limit of 0.6mgkg(-1) laid down for this compound in the Commission Regulation (EU) No 10/2011, so the compliance of the glasses evaluated was ensured. The average recovery percentages of the four analytes at a fortification level of 800ngL(-1) ranged from 50.14 to 92.75%. The detection capability (CCbeta) of the method for BPA was 2.60mugL(-1) for n=2 replicates, with probabilities of false positive and false negative fixed at 0.05.
Descriptors
Links
Book Title
Database
Publisher
Elsevier B.V
Data Source
Authors
Oca,M.L., Sarabia,L.A., Herrero,A., Ortiz,M.C.
Original/Translated Title
URL
Date of Electronic
20140727
PMCID
Editors
N-(4-Fluoro-benzo-yl)-N',N''-diisopropyl-phospho-ric triamide 2012 Department of Chemistry, Ferdowsi University of Mashhad, Mashhad, Iran.
Source Type
Print(0)
Ref Type
Journal Article
Periodical, Full
Acta crystallographica.Section E, Structure reports online
Periodical, Abbrev.
Acta Crystallogr.Sect.E.Struct.Rep.Online
Pub Date Free Form
1-Dec
Volume
68
Issue
Pt 12
Start Page
o3406
Other Pages
7
Notes
LR: 20130418; JID: 101089178; OID: NLM: PMC3588995; 2012/11/06 [received]; 2012/11/09 [accepted]; 2012/11/24 [epublish]; ppublish
Place of Publication
United States
ISSN/ISBN
1600-5368; 1600-5368
Accession Number
PMID: 23476231
Language
eng
SubFile
Journal Article
DOI
10.1107/S1600536812046326 [doi]
Output Language
Unknown(0)
PMID
23476231
Abstract
The asymmetric unit of the title phospho-ric triamide, C13H21FN3O2P, consists of two independent mol-ecules. In each mol-ecule, the P=O group and the N-H unit belonging to the C(O)NHP(O) fragment are in a syn conformation with respect to each other. An intra-molecular N-Hcdots, three dots, centeredO hydrogen bond occurs in each mol-ecule. The P atom adopts a distorted tetra-hedral environment. The methyl groups of an isopropyl fragment are disordered over two sets of sites with refined occupancies of 0.458 (5) and 0.542 (5). In the crystal, mol-ecules are linked through N-Hcdots, three dots, centeredO(=P) and N-Hcdots, three dots, centeredO(=C) hydrogen bonds into chains along [001].
Descriptors
Links
Book Title
Database
Publisher
Data Source
Authors
Pourayoubi,M., Tarahhomi,A., Rheingold,A.L., Golen,J.A.
Original/Translated Title
URL
Date of Electronic
20121124
PMCID
PMC3588995
Editors
Crystal structure of (E)-2-{[(4-anilinophen-yl)imino]-meth-yl}phenol 2015 Department of Chemistry, Indian Institute of Technology Kanpur, Kanpur, UP 208 016, India.; National Taras Shevchenko University, Department of Chemistry, Volodymyrska str. 64, 01601 Kyiv, Ukraine.; National Taras Shevchenko University, Department of Chem
Source Type
Print(0)
Ref Type
Journal Article
Periodical, Full
Acta crystallographica.Section E, Crystallographic communications
Periodical, Abbrev.
Acta Crystallogr.E.Crystallogr.Commun.
Pub Date Free Form
1-Jan
Volume
71
Issue
Pt 1
Start Page
28
Other Pages
30
Notes
LR: 20150225; JID: 101648987; OID: NLM: PMC4331856; OTO: NOTNLM; 2015/01/01 [ecollection]; 2014/11/21 [received]; 2014/11/30 [accepted]; epublish
Place of Publication
England
ISSN/ISBN
2056-9890
Accession Number
PMID: 25705442
Language
eng
SubFile
Journal Article
DOI
10.1107/S2056989014026309 [doi]
Output Language
Unknown(0)
PMID
25705442
Abstract
The title compound, C19H16N2O, crystallized with two independent mol-ecules (A and B) in the asymmetric unit. There is an intra-molecular O-Hcdots, three dots, centeredN hydrogen bond in each mol-ecule with the phenol ring being inclined to the central benzene ring by 4.93 (14) and 7.12 (14) degrees in mol-ecules A and B, respectively. The conformation of the two mol-ecules differs essentially in the orientation of the terminal amino-phenyl ring with respect to the central benzene ring; this dihedral angle is 50.51 (4) degrees in mol-ecule A and 54.61 (14) degrees in mol-ecule B. The two outer aromatic rings are inclined to one another by 51.39 (14) and 49.88 (14) degrees in mol-ecules A and B, respectively. In the crystal, mol-ecules are connected by N-Hcdots, three dots, centeredO hydrogen bonds generating -A-B-A-B- zigzag chains extending along [010]. The chains are linked via C-Hcdots, three dots, centeredpi inter-actions involving neighbouring A mol-ecules, forming slabs lying parallel to (100).
Descriptors
Links
Book Title
Database
Publisher
Data Source
Authors
Faizi,M.S., Iskenderov,T.S., Sharkina,N.O.
Original/Translated Title
URL
Date of Electronic
20150101
PMCID
PMC4331856
Editors
8-{1-[(4'-Fluoro-[1,1'-biphen-yl]-4-yl)meth-yl]piperidin-4-yl}-3,4-di-hydro-quino lin-2(1H)-one chloro-form 0.25-solvate 2014 Department of Chemistry, King Fahad University of Petroleum & Minerals, 31261 Dahran, Saudi Arabia.; Institute of Physics, University of Neuchatel, rue Emile-Argand 11, CH-2000 Neuchatel, Switzerland.
Source Type
Print(0)
Ref Type
Journal Article
Periodical, Full
Acta crystallographica.Section E, Structure reports online
Periodical, Abbrev.
Acta Crystallogr.Sect.E.Struct.Rep.Online
Pub Date Free Form
4-Jan
Volume
70
Issue
Pt 2
Start Page
o103
Other Pages
4
Notes
LR: 20140428; JID: 101089178; OID: NLM: PMC3998275; 2014/02/01 [ecollection]; 2013/12/15 [received]; 2013/12/23 [accepted]; 2014/01/04 [epublish]; epublish
Place of Publication
United States
ISSN/ISBN
1600-5368; 1600-5368
Accession Number
PMID: 24764836
Language
eng
SubFile
Journal Article
DOI
10.1107/S160053681303448X [doi]
Output Language
Unknown(0)
PMID
24764836
Abstract
In the asymmetric unit of the title compound, C27H27FN2O.0.25CHCl3, there are two independent mol-ecules (A and B) together with a partially disordered chloro-form mol-ecule situated about an inversion center. The conformation of the two mol-ecules is very similar. The bridging piperidine rings each have a chair conformation while the piperidin-2-one rings of the quinoline moiety have screw-boat conformations. The benzene rings of the biphenyl moiety are inclined to one another by 26.37 (4) and 23.75 (15) degrees in mol-ecules A and B, respectively. The mean plane of the central piperidine ring [r.m.s. deviation = 0.241 (2) A in both mol-ecules A and B] is inclined to the benzene ring of the quinoline moiety by 80.06 (4) in A and 83.75 (15) degrees in B, while it is inclined to the adjacent benzene ring of the biphenyl group by 73.623 (15) in A and 75.65 (14) degrees in B. In the crystal, individual mol-ecules are linked by pairs of N-Hcdots, three dots, centeredO hydrogen bonds, forming A-A and B-B inversion dimers with R 2 (2)(8) ring motifs. The dimers are stabilized by C-Hcdots, three dots, centeredO hydrogen bonds and linked via C-Hcdots, three dots, centeredF and C-Hcdots, three dots, centeredN hydrogen bonds into a three-dimensional network. Several C-Hcdots, three dots, centeredpi inter-actions are also present.
Descriptors
Links
Book Title
Database
Publisher
Data Source
Authors
Ullah,N., Stoeckli-Evans,H.
Original/Translated Title
URL
Date of Electronic
20140104
PMCID
PMC3998275
Editors
A solid-phase microextraction platinized stainless steel fiber coated with a multiwalled carbon nanotube-polyaniline nanocomposite film for the extraction of thymol and carvacrol in medicinal plants and honey 2015 Department of Chemistry, Lorestan University, Khoramabad, Iran. Electronic address: a_ghiasvand@yahoo.com.; Department of Chemistry, Lorestan University, Khoramabad, Iran.; Department of Chemistry, Lorestan University, Khoramabad, Iran.; Department of Che
Source Type
Print(0)
Ref Type
Journal Article
Periodical, Full
Journal of chromatography.A
Periodical, Abbrev.
J.Chromatogr.A
Pub Date Free Form
7-Aug
Volume
1406
Issue
Start Page
87
Other Pages
93
Notes
CI: Copyright (c) 2015; JID: 9318488; 0 (Aniline Compounds); 0 (Monoterpenes); 0 (Nanotubes, Carbon); 0 (Water Pollutants, Chemical); 0 (polyaniline); 12597-68-1 (Stainless Steel); 3J50XA376E (Thymol); 9B1J4V995Q (carvacrol); OTO: NOTNLM; 2015/04/09 [rece
Place of Publication
Netherlands
ISSN/ISBN
1873-3778; 0021-9673
Accession Number
PMID: 26138604
Language
eng
SubFile
Journal Article; IM
DOI
10.1016/j.chroma.2015.06.052 [doi]
Output Language
Unknown(0)
PMID
26138604
Abstract
A mechanically hard and cohesive porous fiber, with large surface area, for more strong attachment of the coating was provided by platinizing a stainless steel wire. Then, the platinized stainless steel fiber was coated with a multiwalled carbon nanotube/polyaniline (MWCNT/PANI) nanocomposite using electrophoretic deposition (EPD) method and applied for the extraction of thymol and carvacrol with direct-immersion solid-phase microextraction (DI-SPME) method followed by high-performance liquid chromatography-ultraviolet detection (HPLC-UV) quantification. To provide a larger coarse surface for the tightened attachment of coating on the fiber, a stainless steel wire was platinized using a suitable optimized EPD method. Different experimental parameters were studied and the optimal conditions were obtained as: pH of the sample solution: 2; extraction time: 60min; salt content in the sample solution: 1% w/v NaNO3; desorption time: 60min; type and volume of the desorption solvent: acetonitrile, 100muL. Under the optimized conditions, limits of detection (LODs) were 0.6 and 0.8mugmL(-1) for thymol and carvacrol, respectively. Linear dynamic range (LDR) for the calibration curves of both analytes were 1-80mugmL(-1). Relative standard deviation (RSD%, n=6) was 6.8 for thymol and 12.7 for carvacrol. The proposed fiber was successfully applied for the recovery and determination of thymol and carvacrol in thyme, savory, and honey samples.
Descriptors
Links
Book Title
Database
Publisher
Elsevier B.V
Data Source
Authors
Ghiasvand,A., Dowlatshah,S., Nouraei,N., Heidari,N., Yazdankhah,F.
Original/Translated Title
URL
Date of Electronic
20150625
PMCID
Editors
Determination of synthetic polycyclic musks in aqueous samples by ultrasound-assisted dispersive liquid-liquid microextraction and gas chromatography-mass spectrometry 2012 Department of Chemistry, National Central University, Chung-Li 320, Taiwan.
Source Type
Print(0)
Ref Type
Journal Article
Periodical, Full
Analytical and bioanalytical chemistry
Periodical, Abbrev.
Anal.Bioanal Chem.
Pub Date Free Form
Feb
Volume
402
Issue
4
Start Page
1723
Other Pages
1730
Notes
LR: 20160512; JID: 101134327; 0 (Fatty Acids, Monounsaturated); 0 (Water Pollutants, Chemical); 059QF0KO0R (Water); 095I377U8F (musk); 2011/08/07 [received]; 2011/11/11 [accepted]; 2011/11/08 [revised]; 2011/12/04 [aheadofprint]; ppublish
Place of Publication
Germany
ISSN/ISBN
1618-2650; 1618-2642
Accession Number
PMID: 22139524
Language
eng
SubFile
Evaluation Studies; Journal Article; Research Support, Non-U.S. Gov't; IM
DOI
10.1007/s00216-011-5573-3 [doi]
Output Language
Unknown(0)
PMID
22139524
Abstract
A simple and solvent-minimized procedure for the determination of six commonly found synthetic polycyclic musks in aqueous samples using ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) coupled with gas chromatography-mass spectrometry (GC-MS) is described. The parameters affecting the extraction efficiency of analytes from water samples were systematically investigated. The best extraction conditions involved the rapid injection of a mixture of 1.0 mL of isopropyl alcohol (as a dispersant) and 10 muL of carbon tetrachloride (as an extractant) into 10 mL of water containing 0.5 g of sodium chloride in a conical-bottom glass tube. After ultrasonication for 1.0 min and centrifugation at 5,000 rpm (10 min), the sedimented phase 1.0 muL was directly injected into the GC-MS system. The limits of quantitation (LOQs) were less than 0.6 ng/L. The precision for these analytes, as indicated by relative standard deviations (RSDs), was less than 11% for both intra- and interday analysis. Accuracy, expressed as the mean extraction recovery, was between 71 and 104%. Their total concentrations were determined in the range from 8.3 to 63.9 ng/L in various environmental samples by using a standard addition method.
Descriptors
Links
Book Title
Database
Publisher
Data Source
Authors
Yang,C.Y., Ding,W.H.
Original/Translated Title
URL
Date of Electronic
20111204
PMCID
Editors
Purge-assisted headspace solid-phase microextraction combined with gas chromatography/mass spectrometry for the determination of trace nitrated polycyclic aromatic hydrocarbons in aqueous samples 2012 Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan, ROC.
Source Type
Print(0)
Ref Type
Journal Article
Periodical, Full
Journal of chromatography.A
Periodical, Abbrev.
J.Chromatogr.A
Pub Date Free Form
23-Nov
Volume
1265
Issue
Start Page
1
Other Pages
6
Notes
CI: Copyright (c) 2012; JID: 9318488; 0 (Polycyclic Compounds); 0 (Water Pollutants, Chemical); 2012/06/04 [received]; 2012/09/06 [revised]; 2012/09/10 [accepted]; 2012/09/29 [aheadofprint]; ppublish
Place of Publication
Netherlands
ISSN/ISBN
1873-3778; 0021-9673
Accession Number
PMID: 23089518
Language
eng
SubFile
Journal Article; Research Support, Non-U.S. Gov't; IM
DOI
10.1016/j.chroma.2012.09.084 [doi]
Output Language
Unknown(0)
PMID
23089518
Abstract
This study describes a new procedure, namely, purge-assisted headspace solid phase microextraction combined with gas chromatography/negative ion chemical ionization mass spectrometry (PA/HS-SPME-GC/NICI-MS), which is used to determine seven nitrated polycyclic aromatic hydrocarbons (NPAHs) in aqueous samples. High extraction efficiency was obtained with PA/HS-SPME with polydimethylsiloxane (PDMS) fiber coating. A programmable temperature vaporizing (PTV) inlet was used in the desorption process. Selected ion monitoring (SIM) was used for quantitative and qualitative purposes. The linear range of detection of the proposed method was 5-5000 pg/mL with coefficients of determination between 0.995 and 0.999. Limits of detection (LODs) for seven NPAHs were 0.01-0.06 pg/mL. The relative standard deviation was below 12.7% at a concentration of 50 pg/mL. Compared with headspace-solid phase microextraction (HS-SPME), the purge procedure enhanced the extraction efficiency for high boiling point analytes, such as 7-nitrobenz[a]anthracene (7-NBA) and 6-nitrochrysene (6-NC). The proposed method provides a sensitive method for NPAH analysis at the pg/mL level. The application of the proposed method for the determination of trace NPAHs in real samples was investigated by analyzing aqueous samples from rivers. The concentrations of NPAHs detected from the samples ranged from 5.2 to 7.5 pg/mL. This method was applied successfully in the analysis of trace NPAHs in river samples.
Descriptors
Links
Book Title
Database
Publisher
Elsevier B.V
Data Source
Authors
Hung,C.H., Ho,H.P., Lin,M.T., Chen,C.Y., Shu,Y.Y., Lee,M.R.
Original/Translated Title
URL
Date of Electronic
20120929
PMCID
Editors
Determination of benzene, toluene, ethylbenzene, xylenes in water at sub-ng l-1 levels by solid-phase microextraction coupled to cryo-trap gas chromatography-mass spectrometry 2007 Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan, ROC. mrlee@drgon.nchu.edu.tw
Source Type
Print(0)
Ref Type
Journal Article
Periodical, Full
Chemosphere
Periodical, Abbrev.
Chemosphere
Pub Date Free Form
Nov
Volume
69
Issue
9
Start Page
1381
Other Pages
1387
Notes
LR: 20131121; JID: 0320657; 0 (Benzene Derivatives); 0 (Water Pollutants, Chemical); 0 (Xylenes); 3FPU23BG52 (Toluene); J64922108F (Benzene); L5I45M5G0O (ethylbenzene); 2006/12/26 [received]; 2007/05/01 [revised]; 2007/05/03 [accepted]; 2007/06/19 [aheado
Place of Publication
England
ISSN/ISBN
0045-6535; 0045-6535
Accession Number
PMID: 17582460
Language
eng
SubFile
Journal Article; Research Support, Non-U.S. Gov't; IM
DOI
S0045-6535(07)00615-7 [pii]
Output Language
Unknown(0)
PMID
17582460
Abstract
A trace analytical method of benzene, toluene, ethylbenzene and xylenes (BTEX) in water has been developed by using headspace solid-phase microextraction (HS-SPME) coupled to cryo-trap gas chromatography-mass spectrometry (GC-MS). The chromatographic peak shape for BTEX was improved by using cryo-trap equipment. The HS-SPME experimental procedures to extract BTEX from water were optimized with a 75 microm carboxen/polydimethylsiloxane (CAR/PDMS)-coated fiber at a sodium chloride concentration of 267 g l(-1), extraction for 15 min at 25 degrees C and desorption at 290 degrees C for 2 min. Good linearity was verified in a range of 0.0001-50 microg l(-1) for each analyte (r(2)=0.996-0.999). The limits of detection (LODs) of BTEX in water reached at sub-ng l(-1) levels. LODs of benzene, toluene, ethylbenzene, m/p-xylene and o-xylene were 0.04, 0.02, 0.05, 0.01 and 0.02 ng l(-1), respectively. The proposed analytical method was successfully used for the quantification of trace BTEX in ground water. The results indicate that HS-SPME coupled to cryo-trap GC-MS is an effective tool for analysis of BTEX in water samples at the sub-ng l(-1) level.
Descriptors
Benzene/analysis, Benzene Derivatives/analysis, Environmental Monitoring/methods, Freezing, Gas Chromatography-Mass Spectrometry/methods, Reproducibility of Results, Sensitivity and Specificity, Solid Phase Microextraction, Toluene/analysis, Water Pollutants, Chemical/analysis, Xylenes/analysis
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Lee,M. R., Chang,C. M., Dou,J.
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20070619
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