Comparison of two microextraction methods based on solidification of floating organic droplet for the determination of multiclass analytes in river water samples by liquid chromatography tandem mass spectrometry using Central Composite Design

We propose a simple, fast and inexpensive method for the analyses of 72 organic compounds in municipal landfill leachate, based on dispersive liquid-liquid microextraction and comprehensive two-dimensional gas chromatography coupled with mass spectrometry. 41 organic compounds belonging to several classes including hydrocarbons, mono-and polyaromatic hydrocarbons, carbonyl compounds, terpenes, terpenoids, phenols, amines, and phthalates, covering a wide range of physicochemical properties and linked to municipal landfill leachate, were quantitatively determined. Another 31 organic compounds such as indoles, pyrroles, glycols, organophosphate flame retardants, aromatic amines and amides, pharmaceuticals, bisphenol A etc. have been identified based on their mass spectra. The developed method provides good performances in terms of extraction recovery (63.8 -127%), intra-day and inter-day precisions (<7.7 and <13.9 respectively), linearity (R 2 between 0,9669 -0.9999), detection limit (1.01 -69.30 µg L -1 ), quantification limit (1.87 -138.6 µg L -1 ) and 2 enrichment factor (69.6 -138.5). Detailed information on the organic pollutants contained in municipal landfill leachate could be obtained with this method during a 40 minute analysis of a 4 mL leachate sample, using only 75 µL of extraction solvent.

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“…For our purpose EF was calculated based on the following equation (Wang et al 2010;Asati et al 2017;Dil et al 2017):…”

Section: Enrichment Factor and Extraction Recoverymentioning

confidence: 99%

Analysis of multiclass organic pollutant in municipal landfill leachate by dispersive liquid-liquid microextraction and comprehensive two-dimensional gas chromatography coupled with mass spectrometry

Beldean‐Galea

Vial

Thiébaut

et al. 2020

Environ Sci Pollut Res

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“…22 Em relação ao desenvolvimento de metodologias de análise, pesquisadores têm se dedicado à elaboração de métodos de extração que façam uso de solventes como os líquidos iônicos e álcoois de cadeia longa, que além de menos prejudiciais ao meio ambiente, são altamente eficientes no processo de extração de diversos analitos orgânicos. 12,22 No estado de Mato Grosso do Sul (Brasil), boa parte da produção agrícola dos municípios pertencentes à região da Grande Dourados (Caarapó, Douradina, Fátima do Sul, Jateí, Itaporã, Maracaju, Rio Brilhante e Vicentina) ocorre em regiões próximas a Bacia do Rio Dourados. 23 A região produziu em 2017 mais de 2,5 milhões de toneladas de soja e mais de 3,7 milhões de tonelada de milho, sendo que o principal agrotóxico aplicado a essas culturas é o clorpirifós.…”

Section: Artigounclassified

“…11 Alguns artigos publicados recentemente vêm apontando para a presença de clorpirifós em águas fluviais com lavouras próximas, em concentrações variadas, tais como 38,94 μg L -1 ; 1,01 μg L -1 e 2,86 ng L -1 . [12][13][14] Assim, o risco da contaminação de mananciais destinados ao abastecimento de cidades é preocupante, pois, assim como diversas outras substâncias tóxicas, os agrotóxicos não são removidos adequadamente em um sistema de tratamento de água convencional, exigindo processos adicionais mais complexos para que ocorra sua remoção. 15 Dentre as técnicas utilizadas para determinar clorpirifós, assim como outras classes de agrotóxicos, nas mais diversas matrizes, as mais utilizadas são a cromatografia a gás e a líquido.…”

Section: Introductionunclassified

Desenvolvimento De Metodologias Analíticas Para Determinação De Clorpirifós Em Amostras Aquosas Empregando a Microextração Líquido-Líquido Dispersiva Seguida Por HPLC-Uv

Oliveira¹,

Honório²,

Matos³

et al. 2019

Quím. Nova

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Recebido em 15/05/2019; aceito em 27/08/2019; publicado na web em 04/12/2019 DEVELOPMENT OF ANALYTICAL METHODOLOGIES FOR THE DETERMINATION OF CHLORPYRYPHES IN AQUEOUS SAMPLES EMPLOYING THE DISPERSIVE LIQUID MICROEXTRACTION FOLLOWED BY HPLC-UV. The miniaturized extraction techniques use less aggressive methods to the environment, since they generate less waste and spend a minimum of organic solvents, besides having a good selectivity and specificity in the extractions. In this context, liquid-liquid dispersive microextraction (DLLME) has been highlighting. Thus, the present article describes an optimization of the DLLME using low environmental impact extractor solvent to determine the chlorpyrifos insecticide in water. The analytical curves presented values for the correlation coefficient (r) higher than 0.999. The limits of detection and quantification were 0.24 and 0.80 μg L-1 , respectively. There were recoveries between 93 and 97 %, with relative standard deviation (RSD) varying between 1.00 and 3.61%. The developed methods presented accurate and reliable results, are simple and safe, characteristics important for the implementation of a methodology as a routine analysis, and were applied in the determination of chlorpyrifos in water samples from five points along the Rio Dourados, near the city of Fátima do Sul.

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“…However, liquid-liquid Extraction (LLE), solid phase micro extraction (SPME), dispersive liquid-liquid microextraction (DLLME), SPE online, stir bar sorptive extraction (SBSE) are often reported (Farajzadeh & Mogaddam, 2012a;Farajzadeh & Mogaddam, 2012b;Zaater, Tahboub & Sayyed, 2014;Selvaraj et al, 2014;Wu et al, 2015;Caballero-Casero, Lunar & Rubio, 2016;Olatunji et al, 2017;Rozaini et al, 2017;De Araujo, Bauerfeldt & Cid, 2018;Barreca et al, 2019;He & Aga, 2019;Król & Dudziak, 2019). The quantitative analysis is frequently performed by the liquid chromatography coupled to mass spectrometry (LC-MS/MS) and gas chromatography coupled to mass spectrometry (CG-MS) techniques, although other detectors of other kinds coupled to the liquid chromatography are used, such as liquid chromatography with ultraviolet detection (LC-UV), liquid chromatography with diode array detection (LC-DAD) and liquid chromatography with fluorescence detector (LC-FLD) (Zgoła-Grześkowiak et al, 2009;Chen et al, 2010;Lou et al, 2012;Ciofi et al, 2014;Padhye et al, 2014;Camilleri et al, 2015;Terzopoulou, Voutsa & Kaklamanos, 2015;, Asati, Satyanarayana & Patel, 2017;Comtois-Marotte et al, 2017;De Araujo, Bauerfeldt & Cid, 2018. The realization that conventional water and sewage treatment systems do not completely remove most of these micropollutants opens a discussion of a possible worrisome public health problem, since micropollutants may be present in the water supply (Matsuo et al, 2011;Moreira et al, 2011;Silveira et al, 2013;Tran, Hu & Ong, 2013;Dai et al, 2014;Mann et al, 2016;Valls-Cantenys et al, 2016;Tröger et al, 2018;Starling, Amorim & Leão, 2019).…”

Section: Introductionmentioning

confidence: 99%

Development and validation of an analytical method for detection and quantification of benzophenone, bisphenol A, diethyl phthalate and 4-nonylphenol by UPLC-MS/MS in surface water

Araujo

Bauerfeldt

Marques

et al. 2020

PeerJ Analytical Chemistry

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Guandu River is the main water source for 9 million inhabitants in Rio de Janeiro city and some others included in the metropolitan region of the Rio de Janeiro State, Brazil. Here, the development of a chromatographic method and its application to assess the occurrence of 4-nonylphenol (4NP), benzophenone (BP), bisphenol A (BPA) and diethyl-phthalate (DEP), known as endocrine disruptors (EDs), is reported. Sample were prepared by solid phase extraction (SPE) with C18 cartridge and methanol as elution solvent. Validation of analytical method followed the United States Environmental Protection Agency protocol (USEPA 8000D guide) and selectivity, matrix effect, linearity, precision, accuracy, robustness, limit of detection (LOD) and limit of quantification (LOQ) were evaluated. The recovery was greater than 90%, accuracy was found between 80% and 115% and relative standard deviation (RSD) below 11.03%. LOQ ranged from 10.0 to 50.0 ng L−1, while the LOD ranged from 0.87 to 5.72 ng L−1. The coefficients of determination (R2) were greater than 0.99 for all compounds within a linear ranges of 10.0 to 500 ng L−1 for 4NP and BP and 50.0 to 500 ng L−1 for BPA and DEP. The method was therefore considered selective and robust for all micropollutants. Matrix effect was observed for BP, 4NP and DEP. The developed method was applied to analyze five samples collected monthly during 2018 at a selected sampling point of a river in Rio de Janeiro State. The maximum concentrations found for BPA, BP, DEP and 4NP were 182.04, 286.20, 2.56×103 and 13.48 ng L−1 respectively. These values are high enough to justify an investigation on the presence of these micropollutants in drinking water as well as to extend the monitoring for the search of similar pollutants and their metabolites.

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Comparison of two microextraction methods based on solidification of floating organic droplet for the determination of multiclass analytes in river water samples by liquid chromatography tandem mass spectrometry using Central Composite Design

Cited by 33 publications

References 39 publications

Analysis of multiclass organic pollutant in municipal landfill leachate by dispersive liquid-liquid microextraction and comprehensive two-dimensional gas chromatography coupled with mass spectrometry

Analysis of multiclass organic pollutant in municipal landfill leachate by dispersive liquid-liquid microextraction and comprehensive two-dimensional gas chromatography coupled with mass spectrometry

Desenvolvimento De Metodologias Analíticas Para Determinação De Clorpirifós Em Amostras Aquosas Empregando a Microextração Líquido-Líquido Dispersiva Seguida Por HPLC-Uv

Development and validation of an analytical method for detection and quantification of benzophenone, bisphenol A, diethyl phthalate and 4-nonylphenol by UPLC-MS/MS in surface water

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