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Article: Multiresidue Methods for the Determination of Organic Micropollutants and Their Metabolites in Fish Matrices

Molbert, Noëlie / Alliot, Fabrice / Chevreuil, Marc / Goutte, Aurélie / Mouchel, Jean‐Marie / Santos, Raphaël

Environmental toxicology and chemistry. 2019 Sept., v. 38, no. 9

2019

Abstract: Two analytical methods were developed for the determination of 48 organic compounds and 20 of their main by‐products in fish matrices. The targeted compounds belong to various chemical classes of metabolizable (phthalates, polycyclic aromatic ... ...

Abstract	Two analytical methods were developed for the determination of 48 organic compounds and 20 of their main by‐products in fish matrices. The targeted compounds belong to various chemical classes of metabolizable (phthalates, polycyclic aromatic hydrocarbons, insecticides [pyrethroids and N,N‐diethyl‐meta‐toluamide]) and legacy (organochlorine pesticides, polychlorinated biphenyls, polybrominated diphenyl ethers) pollutants. Analyses were performed by gas and liquid chromatography–tandem mass spectrometry in multiple reaction monitoring (MRM) and dynamic MRM, respectively. Method performances were satisfactory, with results meeting the validation criteria because they achieved good linearity responses, recovery, precision, and accuracy for most of the 68 investigated compounds. The methods were then applied on 3 feral chub (Squalius cephalus) collected from the Marne hydrographic network (France). Twenty‐six parent compounds and 5 metabolites were systematically detected in fish matrices, with substantial concentration variability within and among individuals. Phthalates and pyrethroids accounted for most of the pollutant load. Metabolite concentrations in liver samples exceeded those of parent molecules in fish muscle. The present study presents 2 reliable methods for the determination of a wide range of contaminants and underlines the importance of metabolite analysis for a more comprehensive understanding of pollutant bioaccumulation and fate in aquatic organisms. Environ Toxicol Chem 2019;38:1866–1878. © 2019 SETAC.
Keywords	bioaccumulation ; byproducts ; deet ; feral animals ; fish ; insecticides ; liquid chromatography ; liver ; metabolites ; monitoring ; multiresidue analysis ; muscles ; organochlorine pesticides ; phthalates ; pollutants ; pollution load ; polybrominated diphenyl ethers ; polychlorinated biphenyls ; polycyclic aromatic hydrocarbons ; pyrethrins ; Squalius cephalus ; tandem mass spectrometry ; France
Language	English
Dates of publication	2019-09
Size	p. 1866-1878.
Publishing place	John Wiley & Sons, Ltd
Document type	Article
Note	JOURNAL ARTICLE
ZDB-ID	46234-2
ISSN	1552-8618 ; 0730-7268
ISSN (online)	1552-8618
ISSN	0730-7268
DOI	10.1002/etc.4500
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Article ; Online: Multiresidue Methods for the Determination of Organic Micropollutants and Their Metabolites in Fish Matrices.

Molbert, Noëlie / Alliot, Fabrice / Santos, Raphaël / Chevreuil, Marc / Mouchel, Jean-Marie / Goutte, Aurélie

Environmental toxicology and chemistry

2019 Volume 38, Issue 9, Page(s) 1866–1878

Abstract: Two analytical methods were developed for the determination of 48 organic compounds and 20 of their main by-products in fish matrices. The targeted compounds belong to various chemical classes of metabolizable (phthalates, polycyclic aromatic ... ...

Abstract	Two analytical methods were developed for the determination of 48 organic compounds and 20 of their main by-products in fish matrices. The targeted compounds belong to various chemical classes of metabolizable (phthalates, polycyclic aromatic hydrocarbons, insecticides [pyrethroids and N,N-diethyl-meta-toluamide]) and legacy (organochlorine pesticides, polychlorinated biphenyls, polybrominated diphenyl ethers) pollutants. Analyses were performed by gas and liquid chromatography-tandem mass spectrometry in multiple reaction monitoring (MRM) and dynamic MRM, respectively. Method performances were satisfactory, with results meeting the validation criteria because they achieved good linearity responses, recovery, precision, and accuracy for most of the 68 investigated compounds. The methods were then applied on 3 feral chub (Squalius cephalus) collected from the Marne hydrographic network (France). Twenty-six parent compounds and 5 metabolites were systematically detected in fish matrices, with substantial concentration variability within and among individuals. Phthalates and pyrethroids accounted for most of the pollutant load. Metabolite concentrations in liver samples exceeded those of parent molecules in fish muscle. The present study presents 2 reliable methods for the determination of a wide range of contaminants and underlines the importance of metabolite analysis for a more comprehensive understanding of pollutant bioaccumulation and fate in aquatic organisms. Environ Toxicol Chem 2019;38:1866-1878. © 2019 SETAC.
MeSH term(s)	Animals ; Chromatography, Liquid ; Cyprinidae/metabolism ; France ; Insecticides/analysis ; Insecticides/metabolism ; Muscles/chemistry ; Muscles/metabolism ; Organic Chemicals/analysis ; Organic Chemicals/metabolism ; Water Pollutants, Chemical/analysis ; Water Pollutants, Chemical/metabolism
Chemical Substances	Insecticides ; Organic Chemicals ; Water Pollutants, Chemical
Language	English
Publishing date	2019-07-26
Publishing country	United States
Document type	Journal Article ; Research Support, Non-U.S. Gov't
ZDB-ID	46234-2
ISSN	1552-8618 ; 0730-7268
ISSN (online)	1552-8618
ISSN	0730-7268
DOI	10.1002/etc.4500
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Article ; Online: Partitioning behaviour of perfluorinated alkyl contaminants between water, sediment and fish in the Orge River (nearby Paris, France).

Labadie, Pierre / Chevreuil, Marc

Environmental pollution (Barking, Essex : 1987)

2011 Volume 159, Issue 2, Page(s) 391–397

Abstract: This paper reports on the partitioning behaviour of 15 perfluorinated compounds (PFCs), including C(4)-C(10) sulfonates and C(5)-C(14) carboxylic acids, between water, sediment and fish (European chub, Leuciscus cephalus) in the Orge River (nearby Paris). ...

Abstract	This paper reports on the partitioning behaviour of 15 perfluorinated compounds (PFCs), including C(4)-C(10) sulfonates and C(5)-C(14) carboxylic acids, between water, sediment and fish (European chub, Leuciscus cephalus) in the Orge River (nearby Paris). Total PFC levels were 73.0 ± 3.0 ng L(-1) in water and 8.4 ± 0.5 ng g(-1) in sediment. They were in the range 43.1-4997.2 ng g(-1) in fish, in which PFC tissue distribution followed the order plasma > liver > gills > gonads > muscle. Sediment-water distribution coefficients (logK(d)) and bioaccumulation factors (logBAF) were in the range 0.8-4.3 and 0.9-6.7, respectively. Both distribution coefficients positively correlated with perfluoroalkyl chain length. Field-based biota-sediment accumulation factors (BSAFs) are also reported, for the first time for PFCs other than perfluorooctane sulfonate. logBSAF ranged between -1.3 and 1.5 and was negatively correlated with the perfluoroalkyl chain length in the case of carboxylic acids.
MeSH term(s)	Animals ; Cyprinidae/metabolism ; Environmental Monitoring ; Geologic Sediments/analysis ; Gills/chemistry ; Gills/metabolism ; Hydrocarbons, Fluorinated/analysis ; Hydrocarbons, Fluorinated/metabolism ; Liver/chemistry ; Liver/metabolism ; Muscle, Skeletal/chemistry ; Muscle, Skeletal/metabolism ; Paris ; Rivers/chemistry ; Surface-Active Agents/analysis ; Surface-Active Agents/metabolism ; Water Pollutants, Chemical/analysis ; Water Pollutants, Chemical/metabolism
Chemical Substances	Hydrocarbons, Fluorinated ; Surface-Active Agents ; Water Pollutants, Chemical
Language	English
Publishing date	2011-02
Publishing country	England
Document type	Journal Article ; Research Support, Non-U.S. Gov't
ZDB-ID	280652-6
ISSN	1873-6424 ; 0013-9327 ; 0269-7491
ISSN (online)	1873-6424
ISSN	0013-9327 ; 0269-7491
DOI	10.1016/j.envpol.2010.10.039
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Article ; Online: Biogeochemical dynamics of perfluorinated alkyl acids and sulfonates in the River Seine (Paris, France) under contrasting hydrological conditions.

Labadie, Pierre / Chevreuil, Marc

Environmental pollution (Barking, Essex : 1987)

2011 Volume 159, Issue 12, Page(s) 3634–3639

Abstract: The biogeochemical dynamics of 15 perfluorinated compounds (PFCs) were investigated in a heavily urbanised river (River Seine, Paris, France). The target compounds included C4-C10 sulfonates and C5-C14 acids; eleven PFCs were detected and ∑PFCs ranged ... ...

Abstract	The biogeochemical dynamics of 15 perfluorinated compounds (PFCs) were investigated in a heavily urbanised river (River Seine, Paris, France). The target compounds included C4-C10 sulfonates and C5-C14 acids; eleven PFCs were detected and ∑PFCs ranged between 31 and 91 ng L(-1) (median: 47 ng L(-1)). The molecular pattern was dominated by the perfluoroalkyl sulfonates PFHxS and PFOS (>54% of ∑PFCs), which were the only PFCs quantified in both the dissolved and particulate phases. For these PFCs, the sorbed fraction positively correlated with suspended sediment levels. Total PFC levels negatively correlated with river flow rate, which varied between 150 and 640 m(3) s(-1). This suggests the predominance of point sources (likely WWTP effluent discharge), but a contribution of non-point sources such as combined sewer overflow could not be excluded. The annual PFC mass flow was estimated at 500 kg, which is less than observed for other large European rivers.
MeSH term(s)	Alkanesulfonates/analysis ; Environmental Monitoring ; Paris ; Rivers/chemistry ; Water Movements ; Water Pollutants, Chemical/analysis
Chemical Substances	Alkanesulfonates ; Water Pollutants, Chemical
Language	English
Publishing date	2011-12
Publishing country	England
Document type	Journal Article ; Research Support, Non-U.S. Gov't
ZDB-ID	280652-6
ISSN	1873-6424 ; 0013-9327 ; 0269-7491
ISSN (online)	1873-6424
ISSN	0013-9327 ; 0269-7491
DOI	10.1016/j.envpol.2011.07.028
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Article: Partitioning behaviour of perfluorinated alkyl contaminants between water, sediment and fish in the Orge River (nearby Paris, France)

Labadie, Pierre / Chevreuil, Marc

Environmental pollution. 2011 Feb., v. 159, no. 2

2011

Abstract: This paper reports on the partitioning behaviour of 15 perfluorinated compounds (PFCs), including C₄–C₁₀ sulfonates and C₅–C₁₄ carboxylic acids, between water, sediment and fish (European chub, Leuciscus cephalus) in the Orge River (nearby Paris). Total ... ...

Abstract	This paper reports on the partitioning behaviour of 15 perfluorinated compounds (PFCs), including C₄–C₁₀ sulfonates and C₅–C₁₄ carboxylic acids, between water, sediment and fish (European chub, Leuciscus cephalus) in the Orge River (nearby Paris). Total PFC levels were 73.0±3.0ngL⁻¹ in water and 8.4±0.5ngg⁻¹ in sediment. They were in the range 43.1–4997.2ngg⁻¹ in fish, in which PFC tissue distribution followed the order plasma>liver>gills>gonads>muscle. Sediment–water distribution coefficients (logKd) and bioaccumulation factors (logBAF) were in the range 0.8–4.3 and 0.9–6.7, respectively. Both distribution coefficients positively correlated with perfluoroalkyl chain length. Field-based biota–sediment accumulation factors (BSAFs) are also reported, for the first time for PFCs other than perfluorooctane sulfonate. logBSAF ranged between −1.3 and 1.5 and was negatively correlated with the perfluoroalkyl chain length in the case of carboxylic acids.
Keywords	Squalius cephalus ; bioaccumulation ; carboxylic acids ; correlation ; fish ; perfluorocarbons ; rivers ; sediments ; sulfonates ; tissue distribution ; France
Language	English
Dates of publication	2011-02
Size	p. 391-397.
Publishing place	Elsevier Ltd
Document type	Article
ZDB-ID	280652-6
ISSN	1873-6424 ; 0013-9327 ; 0269-7491
ISSN (online)	1873-6424
ISSN	0013-9327 ; 0269-7491
DOI	10.1016/j.envpol.2010.10.039
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Article: Biogeochemical dynamics of perfluorinated alkyl acids and sulfonates in the River Seine (Paris, France) under contrasting hydrological conditions

Labadie, Pierre / Chevreuil, Marc

Environmental pollution. 2011 Dec., v. 159, no. 12

2011

Abstract	The biogeochemical dynamics of 15 perfluorinated compounds (PFCs) were investigated in a heavily urbanised river (River Seine, Paris, France). The target compounds included C4-C10 sulfonates and C5-C14 acids; eleven PFCs were detected and ∑PFCs ranged between 31 and 91 ng L⁻¹ (median: 47 ng L⁻¹). The molecular pattern was dominated by the perfluoroalkyl sulfonates PFHxS and PFOS (>54% of ∑PFCs), which were the only PFCs quantified in both the dissolved and particulate phases. For these PFCs, the sorbed fraction positively correlated with suspended sediment levels. Total PFC levels negatively correlated with river flow rate, which varied between 150 and 640 m³ s⁻¹. This suggests the predominance of point sources (likely WWTP effluent discharge), but a contribution of non-point sources such as combined sewer overflow could not be excluded. The annual PFC mass flow was estimated at 500 kg, which is less than observed for other large European rivers.
Keywords	acids ; correlation ; mass flow ; perfluorocarbons ; rivers ; sulfonates ; suspended sediment ; urbanization ; France
Language	English
Dates of publication	2011-12
Size	p. 3634-3639.
Publishing place	Elsevier Ltd
Document type	Article
ZDB-ID	280652-6
ISSN	1873-6424 ; 0013-9327 ; 0269-7491
ISSN (online)	1873-6424
ISSN	0013-9327 ; 0269-7491
DOI	10.1016/j.envpol.2011.07.028
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Article ; Online: First characterization of the endocrine-disrupting potential of indoor gaseous and particulate contamination: comparison with urban outdoor air (France).

Oziol, Lucie / Alliot, Fabrice / Botton, Jérémie / Bimbot, Maya / Huteau, Viviane / Levi, Yves / Chevreuil, Marc

Environmental science and pollution research international

2017 Volume 24, Issue 3, Page(s) 3142–3152

Abstract: The composition of endocrine-disrupting compounds (EDCs) in the ambient air of indoor environments has already been described, but little is known about the inherent endocrine-disrupting potential of indoor air contamination. We therefore aimed to study ... ...

Abstract	The composition of endocrine-disrupting compounds (EDCs) in the ambient air of indoor environments has already been described, but little is known about the inherent endocrine-disrupting potential of indoor air contamination. We therefore aimed to study the distribution of bioactive EDCs in the gaseous and particulate phases of indoor air using a cellular bioassay approach that integrates the interaction effects between chemicals. Organic air extracts, both gaseous and particulate, were taken from three indoor locations (office, apartment, and children's day care) in France and sampled in two different seasons in order to study their interference with the signaling of estrogen, androgen, and thyroid receptors. The experiments were also conducted on aerial extracts from an outdoor site (urban center). We found that gaseous and/or particulate extracts from all locations displayed estrogenicity, anti-androgenicity, and thyroidicity. Overall, indoor air extracts had a higher endocrine-disrupting potential compared to outdoor ones, especially during winter and in the day care. The biological activities were predominant for the gaseous extracts and tended to increase for the particulate extracts in cool conditions. In conclusion, our data confirmed the presence of bioactive EDCs in a gaseous state and highlighted their indoor origin and concentration, especially in the cold season.
MeSH term(s)	Air Pollutants/analysis ; Air Pollution, Indoor/analysis ; Endocrine Disruptors/analysis ; Environmental Monitoring ; France ; Gases ; Humans ; Particulate Matter/analysis ; Seasons
Chemical Substances	Air Pollutants ; Endocrine Disruptors ; Gases ; Particulate Matter
Language	English
Publishing date	2017-01
Publishing country	Germany
Document type	Journal Article
ZDB-ID	1178791-0
ISSN	1614-7499 ; 0944-1344
ISSN (online)	1614-7499
ISSN	0944-1344
DOI	10.1007/s11356-016-8045-7
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Article ; Online: Trace-Level Determination of Oxolinic Acid and Flumequine in Soil, River Bed Sediment, and River Water Using Microwave-Assisted Extraction and High-Performance Liquid Chromatography with Fluorimetric Detection

Dinh, Quoc Tuc / Nguyễn, Trường Ân / Moreau-Guigon, Elodie / Alliot, Fabrice / Teil, Marie-Jeanne / Blanchard, Martine / Chevreuil, Marc

Soil & sediment contamination. 2017 Apr. 3, v. 26, no. 3 p.247-258

2017

Abstract: This work presents the optimization of analytical procedures for the determination of two antibiotics, oxolinic acid (OA) and flumequine (FL), in bed sediment, river water, and soil samples. Three extraction methods (microwave-assisted extraction (MAE), ... ...

Abstract	This work presents the optimization of analytical procedures for the determination of two antibiotics, oxolinic acid (OA) and flumequine (FL), in bed sediment, river water, and soil samples. Three extraction methods (microwave-assisted extraction (MAE), ultrasonication, and reflux) were tested, and the highest recoveries were obtained with MAE (94 ± 3% and 95 ± 3% for OA and FL, respectively). A solid-phase extraction (SPE) clean-up step was optimized by comparing two polymeric sorbents: Oasis HLB and Oasis MAX. The final extracts were analyzed by liquid chromatography with fluorimetric detection. Limits of detection (LOD) obtained for OA and FL in soil and sediment ranged from 0.3 to 0.5 µg kg ⁻¹. Meanwhile, a novel SPE procedure was also implemented for OA and FL determination in river water samples. It also relied on the use of Oasis MAX, and recovery rates were in the range 90–94%; LODs were 2 ng L ⁻¹ for both OA and FL. These methods were applied for the analysis of samples taken in the Seine River basin (France). The obtained results demonstrated the widespread occurrence of OA and FL, at ng L ⁻¹ and µg kg ⁻¹ levels in water and sediment/soil, respectively, and their persistence in the environment.
Keywords	antibiotics ; detection limit ; flumequine ; fluorometry ; high performance liquid chromatography ; microwave treatment ; oxolinic acid ; river water ; sediments ; soil ; soil sampling ; solid phase extraction ; sorbents ; stream channels ; ultrasonic treatment ; watersheds ; France ; Antibiotics ; sediment ; water ; microwave-assisted extraction ; liquid chromatography/fluorescence
Language	English
Dates of publication	2017-0403
Size	p. 247-258.
Publishing place	Taylor & Francis
Document type	Article ; Online
ZDB-ID	2017739-2
ISSN	1549-7887 ; 1532-0383
ISSN (online)	1549-7887
ISSN	1532-0383
DOI	10.1080/15320383.2017.1276154
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Article: Fate of phthalates and BPA in agricultural and non-agricultural soils of the Paris area (France)

Tran, Bich Chau / Teil, Marie-Jeanne / Blanchard, Martine / Alliot, Fabrice / Chevreuil, Marc

Environmental science and pollution research international. 2015 July, v. 22, no. 14

2015

Abstract: This study (i) investigated the concentration levels of nine phthalates and bisphenol A (BPA) in sludge samples originating from a French wastewater treatment plant (WWTP), (ii) studied the distribution of target compounds according to soil depth and ... ...

Abstract	This study (i) investigated the concentration levels of nine phthalates and bisphenol A (BPA) in sludge samples originating from a French wastewater treatment plant (WWTP), (ii) studied the distribution of target compounds according to soil depth and calculated their half-lives, and (iii) compared the contamination level of the agricultural soil with those of soils with other land uses. The sludge contamination levels varied from a few hundred nanograms per gram dry weight (dw) for diethyl phthalate (DEP), di-iso-butyl phthalate (DiBP), di-n-butyl phthalate (DnBP), and butyl-benzyl phthalate (BBP) to a few micrograms per gram dw for diethylhexyl phthalate (DEHP), di-iso-nonyl phthalate (DiNP), and di-iso-decyl phthalate (DiDP). After sludge application, an 8-fold increase for DEHP level and a 3-fold increase for BPA level occurred in the surface horizon of the soil. The mean distribution of phthalates according to the depth showed a positive gradient for the low molecular weight compounds and inversely, a negative gradient for the highest ones. The half-lives in the 0–20-cm soil horizon were 64 days for DEHP and 36 days for BPA. A predictive environmental concentration (PEC) of 0.3 μg g⁻¹ dw was estimated for DEHP, while the experimental value was 0.16 μg g⁻¹ dw, suggesting degradation processes in soil and/or formation of non-extractable residues. Comparisons of contamination levels for soils from different origins (urban, rural, agricultural, and forest) showed that the urban soil remained the most contaminated one, prior to the agricultural soil after treatment.
Keywords	agricultural soils ; bisphenol A ; forests ; half life ; land use ; molecular weight ; phthalates ; sludge ; soil depth ; soil horizons ; urban soils ; wastewater treatment ; France
Language	English
Dates of publication	2015-07
Size	p. 11118-11126.
Publishing place	Springer Berlin Heidelberg
Document type	Article
ZDB-ID	1178791-0
ISSN	1614-7499 ; 0944-1344
ISSN (online)	1614-7499
ISSN	0944-1344
DOI	10.1007/s11356-015-4178-3
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Article ; Online: A new analytical protocol for the determination of 62 endocrine-disrupting compounds in indoor air.

Laborie, Stéphanie / Moreau-Guigon, Elodie / Alliot, Fabrice / Desportes, Annie / Oziol, Lucie / Chevreuil, Marc

Talanta

2016 Volume 147, Page(s) 132–141

Abstract: The objective of this study was to develop and validate a new analytical protocol for simultaneous determination of 62 semi-volatile organic compounds in both phases of indoor air. Studied compounds belong to several families: polybrominated diphenyl ... ...

Abstract	The objective of this study was to develop and validate a new analytical protocol for simultaneous determination of 62 semi-volatile organic compounds in both phases of indoor air. Studied compounds belong to several families: polybrominated diphenyl ethers, polychlorinated biphenyls, hexachlorobenzene, pentachlorobenzene, phthalates, polyaromatic hydrocarbons, parabens, tetrabromobisphenol A, bisphenol A, hexabromocyclododecane, triclosan, alkylphenols, alkylphenol ethoxylates, synthetic musks (galaxolide and tonalide) and pesticides (lindane and cypermethrin). A medium volume sampling system was used to collect simultaneously these endocrine-disrupting compounds (EDCs) from the gaseous and particulate phases. An accelerated solvent extraction method was optimized to obtain all EDCs in a single extract by atmospheric phase. Their extraction from the sorbents and their analysis by liquid and gas chromatography-mass spectrometry (LC/MS/MS, GC/MS and GC/MS/MS) was validated using spiked sorbents (recovery study and analytical uncertainty analysis by fully nested design). The developed protocol achieved low limits of quantification (<0.5ng m(-3)) and low uncertainty values (<5ng m(-3)) for all compounds. Once validated, the method was applied to indoor air samples from four locations (a house, an apartment, a day nursery and an office) and compared to literature to confirm its efficiency. All target EDCs were quantified in the samples and were primarily present in the gaseous phase. The major contaminants found in indoor air were, in descending order, phthalates, synthetic musks, alkylphenols and parabens.
MeSH term(s)	Air Pollution, Indoor/analysis ; Chemistry Techniques, Analytical/methods ; Chromatography, Liquid ; Endocrine Disruptors/analysis ; Endocrine Disruptors/chemistry ; Environmental Monitoring/methods ; Gas Chromatography-Mass Spectrometry
Chemical Substances	Endocrine Disruptors
Language	English
Publishing date	2016-01-15
Publishing country	Netherlands
Document type	Journal Article ; Research Support, Non-U.S. Gov't
ZDB-ID	1500969-5
ISSN	1873-3573 ; 0039-9140
ISSN (online)	1873-3573
ISSN	0039-9140
DOI	10.1016/j.talanta.2015.09.028
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