Determination of chlorinated pesticides in water by SPME/GC

Boussahel, R.; Bouland, S.; Moussaoui, Khadija M.; Baudu, Michel; Montiel, Altamira Díaz

doi:10.1016/s0043-1354(01)00372-4

Cited by 46 publications

(18 citation statements)

References 9 publications

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“…Esta técnica puede automatizarse y es empleada para el aislamiento de compuestos orgánicos de muestras acuosas o de una fase gaseosa (Alpendurada 2000, Boussahel et al 2002, Nollet 2006. Además puede realizarse empleando pequeñas cantidades de muestra.…”

Section: Microextracción En Fase Sólida (Spme)unclassified

“…En agua de consumo humano, se han probado técnicas como la SPME y la SDME, que simplifican el proceso de separación, al disminuir los tiempos de partición y eliminar la etapa de limpieza del extracto; se pueden reducir costos y residuos aumentando la efectividad en los límites de detección y reproducibilidad (Cuadro IV) (Alpendurada 2000, Boussahel et al 2002, López-Blanco et al 2003, Beceiro-González et al 2007, Wang et al 2008. SC: sistema cromatográfico, LD: límite de detección, LC: límite de cuantificación, GC-ECD: Cromatografía de gases con detector de captura de electrones, GC-MS: Cromatografía de gases acoplamiento a espectrometría de masas, %R: porcentaje de recuperación P.E.…”

Section: Comparación De Técnicas De Extracción Y Limpiezaunclassified

“…La precisión, muy pocas investigaciones la reportaron a través del coeficiente de variación (CV) para las repeticiones de las determinaciones. Los valores encontrados fueron CV de 1.7 a 13.06 (Boussahel et al 2002, López-Blanco et al 2003, Lorenzatti et al 2003, Ramírez, 2009). …”

Section: Cromatografía De Gases Acoplado a Espectrometría De Masas (Gunclassified

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Métodos Cromatográficos Para La Determinación De Endosulfán en Alimentos

Ángeles-Hernández

Amaya-Chávez

Rivera

et al. 2018

Rev. Int. Contam. Ambie.

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Palabras clave: plaguicidas orgánicos persistentes, extracción y limpieza, metodología analítica RESUMEN Se revisaron las técnicas de extracción, limpieza y cuantificación de endosulfán por métodos cromatográficos en matrices alimentarias como productos lácteos, frutas y vegetales, así como pescados y mariscos, publicados en los últimos veinte años. Independientemente del tipo de matriz, su extracción se realiza principalmente con disolventes orgánicos como hexano, metanol, acetonitrilo y acetona. Para la limpieza, lo más comúnmente empleado fueron cartuchos de sílice, columnas de florisil, o C18. En cuanto a la cuantificación, el método más sensible resultó ser la cromatografía de gases acoplada a espectrofotometría de masas (CG-MS). Los alimentos en los que se reportó la presencia de α, β y/o sulfato de endosulfán fueron: productos lácteos y sus derivados con un intervalo de concentraciones de 23.99 a 52.2 ng/g; pescados y mariscos de 1.07 a 49.7 ng/g; y vegetales de 0.5 a 5460.0 ng/g. En leche materna se reportaron concentraciones de 0.4 a 10.7 ng/mL y en grasa hasta 277.39 ng/g. Keywords: persistent organic pesticides, extraction and cleaning, analytic methodology ABSTRACT Extraction and cleaning techniques plus chromatographic methods were reviewed for the quantification of endosulfan in food matrices such as dairy products, fruits and vegetables, fish and seafood, published in the last twenty years. Regardless of the type of matrix, the extraction of endosulfan is carried out mainly with organic solvents such as hexane, methanol, acetonitrile and acetone. For cleaning, the most common was the use silica cartridges, florisil columns, or C18. The most sensitive quantification method was gas chromatography coupled to mass spectrometry (GC-MS. Foods where it was reported the presence of α, β and/or endosulfan sulfate were dairy products and their derivatives in a range of 23.99 to 52.2 ng/g, in fish and shellfish from 1.07 to 49.7 ng/g, vegetables from 0.5 to 5460.0 ng/g. In breast milk were from 0.4 to 10.7 ng/mL and in fat until 277.39 ng/g. REVISIÓNRev. Int. Contam. Ambie. 34 (Especial sobre Contaminación y Toxicología por Plaguicidas (CTP) [81][82][83][84][85][86][87][88][89][90][91][92][93][94] 2018

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Section: Microextracción En Fase Sólida (Spme)unclassified

Section: Comparación De Técnicas De Extracción Y Limpiezaunclassified

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Métodos Cromatográficos Para La Determinación De Endosulfán en Alimentos

Ángeles-Hernández

Amaya-Chávez

Rivera

et al. 2018

Rev. Int. Contam. Ambie.

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“…11,12 The application of SPME for retention of pesticides has been reported in various matrices including soil, 8 food, 13,14 river water, 15 rain water, 16 raw and treated water, 17 groundwater 18,19 and aqueous matrizes. [20][21][22][23][24][25][26] The technique consists in the extraction of analytes using a silica fiber coated with a layer of sorbent, which is exposed directly in the sample or in the headspace. After the equilibrium time has been reached, the fiber is introduced into the chromatographic system for desorption of the analytes.…”

Section: Introductionmentioning

confidence: 99%

Multiresidue methods for determination of pesticides using SPME and SPE followed by GC-NPD system: a comparative study

Milhome

Sousa

Keukeleire

et al. 2011

J. Braz. Chem. Soc.

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Neste estudo, métodos multirresíduos usando extração em fase sólida (SPE) e microextração em fase sólida (SPME) são comparados na determinação de pesticidas em amostras aquosas. Parâmetros como tipo de fibras e espessura, solvente de eluição, volume da amostra, tempo de equilíbrio, coeficiente de partição e solubilidade foram investigados. Resultados satisfatórios foram obtidos para a análise de pesticidas usando cartuchos C18 e acetato de etila como eluente, com taxas de recuperação entre 75-107%. As melhores condições para SPME foram com uma fibra PDMS 100 µm de espessura, volume de amostra de 40 mL, e tempo de equilíbrio de 45 min. O método SPME é o mais adequado para a análise de pesticidas em água, devido à sua rapidez e simplicidade e ao não uso de solventes. Os limites de detecção e quantificação são inferiores aos limites de concentração máximos estabelecidos pelas autoridades brasileiras, sendo portanto aceitável.In this study, multiresidue method using solid phase extraction (SPE) and solid phase microextraction (SPME) are compared in the determination of pesticides in aqueous samples. Parameters such as fiber type and thickness, elution solvent, sample volume, equilibration time, partition coefficient and solubility were investigated. Satisfactory results were obtained for the analysis of pesticides using C18 cartridges and ethyl acetate as eluent, whith recovery rates between 75-107%. The best conditions for SPME fiber were PDMS with a 100 mm thick, sample volume of 40 mL, and reaction time was 45 min. SPME method is most suitable for the analysis of pesticides in water, due to its speed and simplicity and solvent-free. The limits of detection and quantification are below the maximum concentration limits established by Brazilian authorities and therefore acceptable.Keywords: pesticides, SPME, water analysis, microextraction, partition coefficient IntroductionThe protection of water quality is a real concern of government agencies that control public health. The worldwide intensive use of pesticides plays a key role in environmental contamination, especially in water resources. In the last years, Brazil has been considered the largest consumer of pesticides in the world. 1 Only in 2009, around 1 million ton of pesticides were sold in the country,mainly applied in soybean, corn, sugarcane and cotton cultures. 1 According to ANDEF, there were about 475 active ingredients and 1278 products registered. 2 Pesticides that remain in the environment or reach the aquatic systems pose risks to animal species by their toxicity and ability to bio-accumulate along the food chain. 3 The European Community has set the value of 0.1 mg L -1 for any individual pesticide and 0.5 mg L -1 for the total pesticide residues of pesticides. In Brazil, the maximum concentrations of pesticides in water are regulated by the Administrative Rule No. 518/2004 (drinking water) of the Milhome et al. 2049 Vol. 22, No. 11, 2011 Ministry of Health, by The National Environment Council (CONAMA) Resolution No. 357/2005(classification o...

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“…sorptive extraction, RDSE), 14 고체상 미량추출법(solid phase microextraction, SPME), 15,30 고체상 추출법(solid phase extraction, SPE), 15,18,20,21,23,24,26,32 단일 방울 미량추출법(single-drop microextraction, SDME), 16 직접 담금 고체상 미량추출법(direct immersion, DI)-SPME, 17,19 직접 주입법(direct injection, DI),…”

mentioning

confidence: 99%

Simultaneous Determination of Ultra-Trace Pesticides and Synthetic Materials in Surface Water by LC-ESI-MS/MS

Hong¹,

Lee²,

Lee³

et al. 2015

Journal of the Korean Chemical Society

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주제어: 농약, 합성원료, 하천수, 고체상 추출, 액체크로마토그래피 텐덤 질량분석법ABSTRACT. A liquid chromatography-electrospray ionization-tandem mass spectrometry method (LC-ESI-MS/MS) was used for determining seven pesticides (2,4-dichlorophenoxyacetic acid, methomyl, aldicarb, 2-methyl-4-chlorophenoxy-acetic acid, molinate, carbaryl and carbofuran) and two synthetic materials (quinoline and bisphenol-A) in surface water. The analytes were extracted using solid-phase extraction (SPE). The eluate was concentrated by nitrogen gas. 100 microliters of 30% (v/v) methanol aqueous solution were used to dissolve the residue and an aliquot of the reconstituted solution was directly injected into LC-ESI-MS/MS after the filtration using 0.2 μm polytetrafluoroethylene (PTFE) syringe filter. Under the established condition, the calibration curves of the analytes were linear with correlation coefficients of above 0.997. The quantification limit was 0.002~0.011 μg/L and the relative standard deviations were less than 16.4%. In addition, accuracy was in the range of 84~107% and the recoveries were values between 56.2 and 98.6%. In this study, the developed method was applied to the analysis of real surface water samples.

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Determination of chlorinated pesticides in water by SPME/GC

Cited by 46 publications

References 9 publications

Métodos Cromatográficos Para La Determinación De Endosulfán en Alimentos

Métodos Cromatográficos Para La Determinación De Endosulfán en Alimentos

Multiresidue methods for determination of pesticides using SPME and SPE followed by GC-NPD system: a comparative study

Simultaneous Determination of Ultra-Trace Pesticides and Synthetic Materials in Surface Water by LC-ESI-MS/MS

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