Solid phase microextraction gas chromatographic analysis of organophosphorus pesticides in biological samples

Tsoukali, Heleni; Theodoridis, Georgios; Raikos, Νikolaos; Grigoratou, Ifigeneia

doi:10.1016/j.jchromb.2005.05.035

Cited by 80 publications

(40 citation statements)

References 18 publications

(37 reference statements)

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“…The electroactive areas of both bare bppg and graphitebppg electrodes were obtained by cyclic voltammetry (CV) using K 3 [Fe(CN) 6 ] as a probe at different scan rates in 25 °C. For a reversible process at 25 °C , the RandlesSevcik formula has been used:…”

Section: Preparation and Modification Of The Electrodementioning

confidence: 99%

“…[5][6][7][8][9][10][11][12][13] Although chromatography techniques have been widely applied, they are time-consuming, solvent-usage intensive, require expensive equipment and maintenance, and often result in a lengthy turnaround of pretreatment steps. For all these reasons, the faster and more economic electrochemical detection of pesticides including OPs is a very desirable.…”

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confidence: 99%

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Electrochemical feasibility study of methyl parathion determination on graphite-modified basal plane pyrolytic graphite electrode

Okumura¹,

Saczk²,

Oliveira³

et al. 2011

J. Braz. Chem. Soc.

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Um método eletroquímico de baixo custo foi desenvolvido para a determinação de traços de metil paration (MP) baseado nas propriedades do eletrodo de grafite pirolítico de plano basal modificado com grafite (grafite-bppg). A combinação do grafite-bppg com voltametria de onda quadrada (VOQ) resultou em um método eletroquímico seletivo, sensível e original para a determinação do pesticida MP em água potável. O eletrodo foi construído e o comportamento eletroquímico do MP foi estudado. A imobilização foi feita através de modificação por formação de filme a partir da dispersão de pó de grafite em água destilada e através de pipetagem de um volume pequeno sobre a superfície do eletrodo, permitindo que o solvente volatilizasse. A forte afinidade do modificador grafite com o grupo fósforo do MP permitiu o depósito de uma quantidade significativa de MP em menos de 60 segundos. Os resultados de voltametria cíclica mostraram que o eletrodo de grafite-bppg pode aumentar a sensibilidade na intensidade de corrente para os picos redox quasi-reversíveis dos produtos da redução catódica do grupo nitro em potencial negativo (pico I = 0,077 V e o pico II = -0,062 V) e para o pico catódico irreversível (pico III = -0,586 V) em comparação com o eletrodo não modificado bppg e que o processo é também controlado por adsorção. Sob condições otimizadas, o intervalo de concentração e limite de detecção para o pesticida MP são 79,0 a 263,3 mmol L -1 e 3,00 mmol L -1 , respectivamente. O método proposto foi aplicado com sucesso à determinação do MP em água potável e o desempenho deste sensor eletroquímico foi avaliado em termos de figuras de mérito analíticas.A low-cost electrochemical method was developed for the determination of trace-level of methyl parathion (MP) based on the properties of graphite-modified basal plane pyrolytic graphite electrode (graphite-bppg). A combination of graphite-bppg with square-wave voltammetric (SWV) analysis resulted in an original, sensitive and selective electrochemical method for determination of MP pesticide in drinking water. The electrode was constructed and the electrochemical behavior of MP was studied. Immobilization is achieved via film modification from dispersing graphite powder in deionized water and through pipeting a small volume onto the electrode surface allowing the solvent to volatilize. The strong affinity of the graphite modifier for the phosphorous group of the MP allowed the deposition of a significant amount of MP in less than 60 seconds. The cyclic voltammetric results indicate that the graphite-bppg electrode can enhance sensitivity in current intensity towards the quasi-reversible redox peaks of the products of the cathodic reduction of the nitro group at negative potential (peak I = 0.077 V and peak II = -0.062 V) and that the cathodic irreversible peak (peak III = -0.586 V) in comparison with bare bppg electrode and is also adsorption controlled process. Under optimized conditions, the concentration range and detection limit for MP pesticide are respectively 79.0 to 263.3 mmol ...

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Section: Preparation and Modification Of The Electrodementioning

confidence: 99%

mentioning

confidence: 99%

Electrochemical feasibility study of methyl parathion determination on graphite-modified basal plane pyrolytic graphite electrode

Okumura¹,

Saczk²,

Oliveira³

et al. 2011

J. Braz. Chem. Soc.

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“…Tsoukali et coll. [11] publient une méthode alliant la SPME à la GC-NPD (détecteur azote phosphore). Le plasma additionné de l'étalon interne (fénitrothion) et de NaCl est dilué dans un petit volume d'eau distillée.…”

Section: Organophosphorés (Op)unclassified

Difficultés analytiques de la caractérisation des pesticides dans le sang

Anger

Kintz²

2009

Ann Toxicol Anal

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Résumé -Objectifs : Malgré les incontestables services qu'ils ont pu rendre à l'agriculture, l'utilisation des pesticides n'est pas sans danger pour l'homme. En dehors des intoxications aiguës accidentelles ou volontaires, l'exposition répétée à ces produits ou la consommation d'aliments contaminés par leurs résidus peuvent être à l'origine de divers troubles pour la santé humaine : perturbations endocriniennes, dérèglement du système immunitaire, apparition de certains types de cancers, troubles de la reproduction, etc. Il importe donc de pouvoir les caractériser ou surveiller leur présence dans les milieux biologiques. L'objet de ce travail est de recenser les moyens analytiques modernes qui permettent de doser les pesticides dans le sang, milieu biologique facilement accessible et de composition constante et d'insister sur les difficultés analytiques rencontrées lors du choix de la méthode et de l'interprétation des résultats. Méthodes : De très nombreuses techniques analytiques sont proposées aujourd'hui pour l'analyse des pesticides et/ou leurs métabolites dans les milieux biologiques. Après traitement de l'échantillon, le plus souvent par micro-extraction en phase solide (SPME), l'analyse instrumentale proprement dite fait appel aux méthodes chromatographiques classiques comme la chromatographie en phase gazeuse (GC) ou la chromatographie liquide haute performance (HPLC) couplées toutes deux à la spectrométrie de masse simple (MS) ou en tandem (MS/MS). Certaines méthodes permettent la caractérisation de plusieurs pesticides appartenant à des familles différentes, mais elles restent rares. La plupart des techniques se limitent à doser un groupe donné de pesticides dans des conditions expérimentales bien précises. Ré-sultats : La mise en évidence des pesticides dans le sang requiert des techniques sophistiquées nécessitant un matériel souvent onéreux et des techniciens expérimentés. Les concentrations toxiques sont très variables d'un composé à l'autre et justifient la recherche d'une limite de quantification (LOQ) parfois très faible. L'obtention d'étalons de référence purs peut également être source de difficultés sans compter qu'il n'existe pas de méthode officielle recommandée. L'interprétation des résultats constitue sans doute le problème majeur car la toxicocinétique des pesticides est généralement mal connue et difficile à établir chez l'homme. Conclusions et perspectives : Il n'existe pas aujourd'hui de méthode universelle de dosage des pesticides dans le sang. La mise en place d'une méthodologie donnée requiert une demande bien précise de la part du clinicien. L'interprétation des résultats reste parfois difficile. Il apparaît donc évident que le développement d'un screening général de recherche des pesticides comme il en existe un actuellement pour les médica-ments, puisse voir le jour afin de raccourcir le délai de réponse du laboratoire au clinicien. L'immunochimie apportera peut-être la solution. Mots clés : Pesticide, environnementAbstract -Objectives: Despite the undoubted services which they...

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“…Moreover, Direct Immersion (DI)-SPME-GC-MS technique has been performed for determining the chlorpyrifos in water samples [29]. HS-SPME procedure has been applied for pesticide's purification in biological samples such as chloraacetanilide [30] and organophosphorus pesticides [31].…”

Section: Introductionmentioning

confidence: 99%

Optimization of Solid Phase Microextraction Procedure Followed by Gas Chromatography with Electron Capture Detector for Pesticides Butachlor and Chlorpyrifos

Ghavidel¹,

Shahtaheri²,

Jazani³

et al. 2014

AJAC

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In this study, headspace solid phase microextraction (HS-SPME) followed by gas chromatography using electron capture detection system (GC-ECD) were developed for the determination of chloraacetanilide (butachlor) and chlorpyrifos presented in biological samples. Different parameters affecting the extraction procedure were optimized including extraction time (30 minutes), extraction temperature (80˚C), sample volume (3 mL), sample pH (2), added NaCl (0.3 gram) and sample stirring rate (400 rpm). Different concentrations of 1 -100 ng/ml were applied for butachlor and a linear calibration curve was obtained. Furthermore, a similar linearity was obtained for chlorpyrifos, using a concentration range of 1 -250 ng/ml. The limit of detection (LOD) obtained for butachlor and chlorpyrifos were 0.088 and 0.53 ng/ml respectively. The optimized methods for both compounds were validated using two concentrations of 25 and 50 ng/ml in spiked urine samples. Obtained recoveries of spiked urine samples were 83.06% -99.8% with RSD of lower than 11%. Optimized technique was simple, inexpensive, solvent free and fast in comparison with other conventional methods and had compatibility with the chromatographic analytical system. This method offers low detection limits to analyze pesticides in urine samples that are very important * Corresponding author. F. Ghavidel et al. 536in the exposure monitoring in occupational health.

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Solid phase microextraction gas chromatographic analysis of organophosphorus pesticides in biological samples

Cited by 80 publications

References 18 publications

Electrochemical feasibility study of methyl parathion determination on graphite-modified basal plane pyrolytic graphite electrode

Electrochemical feasibility study of methyl parathion determination on graphite-modified basal plane pyrolytic graphite electrode

Difficultés analytiques de la caractérisation des pesticides dans le sang

Optimization of Solid Phase Microextraction Procedure Followed by Gas Chromatography with Electron Capture Detector for Pesticides Butachlor and Chlorpyrifos

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