Ultrasound-vortex-assisted dispersive liquid–liquid microextraction coupled with gas chromatography with a nitrogen–phosphorus detector for simultaneous and rapid determination of organophosphorus pesticides and triazines in wine

Cinelli, Giuseppe; Avino, Pasquale; Notardonato, Ivan; Russo, Mario Vincenzo

doi:10.1039/c3ay41641k

Cited by 62 publications

(29 citation statements)

References 44 publications

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“…11,12 Quando a mistura tolueno:água é submetida ao ultrassom ocorre a formação de micro gotículas de tolueno que se dispersam rapidamente na água. Este fenômeno pode ser percebido visualmente pela turvação da mistura formada durante os experimentos.…”

Section: Avaliação Da Temperatura E Tempo De Sonicaçãounclassified

“…9 Mais recentemente, também tem sido destacada a eficácia da microextração líquido-líquido com dispersão assistida por agitação em vortex e ultrassom (USVADLLME -ultrasound vortex assisted dispersive liquid-liquid microextraction) na determinação de diversos analitos em matrizes aquosas, como refrigerantes e bebidas alcoólicas por cromatografia em fase gasosa. 10,11 A agitação em vortex e a radiação ultrassônica intensificam o processo de dispersão do solvente extrator e contribuem para aumentar a superfície de contato entre a fase orgânica (solvente extrator) e a fase aquosa, o que favorece a partição dos compostos de interesse entre as duas fases imiscíveis. [13][14][15] Com isso, a USVADLLME pode suprimir a utilização do solvente dispersor e resolver um problema clássico da DLLME, que é a solubilização do solvente extrator na amostra devido a este solvente.…”

Section: Introductionunclassified

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Ultrasound Vortex Assisted Dispersive Liquid-Liquid Microextraction (Usvadllme) Applied to the Determination of the Triazole Flutriafol and Triazines and Triazinones Pesticides in Water

Duarte¹,

Dores²,

Villa³

2016

Química Nova

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Recebido em 16/12/2015; aceito em 18/04/2016; publicado na web em 17/06/2016 ULTRASOUND VORTEX ASSISTED DISPERSIVE LIQUID-LIQUID MICROEXTRACTION (USVADLLME) APPLIED TO THE DETERMINATION OF THE TRIAZOLE FLUTRIAFOL AND TRIAZINES AND TRIAZINONES PESTICIDES IN WATER. This study aimed at developing and validating a method for the simultaneous determination of triazines (ametryne, atrazine, prometryne and terbuthylazine), triazinones (metribuzin and hexazinone) and a triazole (flutriafol) in water by ultrasound vortex assisted dispersive liquid-liquid microextraction (USVADLLME) and GC-MS. The experimental conditions that provided the best results were: 5.00 mL of sample, 100 mL of extractor solvent (toluene), vortex agitation for 30 s and sonication for 1 min. at 240 W and 40 °C. The USVADLLME provided recoveries ranging from 77.2% to 109%, with a repetitivity and intermediate precision varying from 1.4 to 9.0% and 2.9 to 15%, respectively. The method detection limits ranged between 0.10 and 2.71 µg L -1. The method was applied to different surface water samples and a matrix effect was not observed. Once validated, the proposed method was applied to ten water samples of an important agricultural region of Mato Grosso State/Brazil, but none of the studied analytes were detected. The USVADLLME is proposed as an efficient, fast, simple and non-expensive alternative technique for the simultaneous determination of multiclass pesticides in water.Keywords: method validation; herbicides; gas chromatography. INTRODUÇÃOAs triazinas e as triazinonas estão dentre as classes de herbicidas mais utilizadas no mundo, principalmente no controle seletivo de ervas daninhas de folha larga e gramíneas em lavouras de milho, soja e algodão. A preocupação com a persistência, mobilidade e a toxicidade destes agrotóxicos tem sido crescente, devido à detecção dos mesmos em águas subterrâneas e em diferentes compartimentos ambientais. 1,2 O triazol flutriafol possui uma ampla atividade fungicida e também é muito utilizado em culturas de cereais. Embora seja considerado de baixa toxicidade, o flutriafol é extremamente persistente no solo com um elevado potencial de mobilidade e, portanto, um potencial contaminante de águas subterráneas.3 A contaminação de recursos hídricos por agrotóxicos tem sido objeto de grande preocupação mundial e motivado o desenvolvimento de diversos métodos analíticos para a determinação destes compostos em água. [4][5][6] A diversidade de princípios ativos bem como as diferentes características físico-químicas do material a ser analisado são alguns dos fatores que podem limitar a aplicabilidade de muitos destes métodos. Além disso, para determinadas finalidades são necessários métodos com baixos limites de detecção, da ordem de ng L -1 , o que pode requerer etapas de extração e pré-concentração dos analitos. Estas etapas estão dentre as mais críticas do processo, pois delas dependem a exatidão, a precisão e o limite de detecção do método.A extração líquido-líquido (LLE -Liquid-Liquid Extraction) e extração em fase sólid...

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Section: Avaliação Da Temperatura E Tempo De Sonicaçãounclassified

Section: Introductionunclassified

Ultrasound Vortex Assisted Dispersive Liquid-Liquid Microextraction (Usvadllme) Applied to the Determination of the Triazole Flutriafol and Triazines and Triazinones Pesticides in Water

Duarte¹,

Dores²,

Villa³

2016

Química Nova

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“…This problem can be avoided by using ultrasonic stirring or a cationic surfactant in order to disperse the extraction solvent instead of dispersive solvent. In order to help the dispersion process, vortex agitation is also used [40][41][42]. Additionally, new solutions and improvements of the DLLME technique have recently been proposed.…”

Section: Introductionmentioning

confidence: 99%

“…In order to remove the centrifugation step, which is considered as one of the most time-consuming steps in this method, demulsified DLLME has been proposed [40][41][42]. After the introduction of the solvent mixture and consequently emulsion formation, another portion of dispersive solvent (serving as demulsifier) is introduced, leading to the breakup of the emulsion.…”

Section: Introductionmentioning

confidence: 99%

Fast, sensitive and reliable multi-residue method for routine determination of 34 pesticides from various chemical groups in water samples by using dispersive liquid–liquid microextraction coupled with gas chromatography–mass spectrometry

Tankiewicz

Biziuk

2017

Anal Bioanal Chem

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A simple and efficient dispersive liquid-liquid microextraction technique (DLLME) was developed by using a mixture of two solvents: 40 μL of tetrachlorethylene (extraction solvent) and 1.0 mL of methanol (disperser solvent), which was rapidly injected with a syringe into 10 mL of water sample. Some important parameters affecting the extraction efficiency, such as type and volume of solvents, water sample volume, extraction time, temperature, pH adjustment and salt addition effect were investigated. Simultaneous determination of 34 commonly used pesticides was performed by using gas chromatography coupled with mass spectrometry (GC-MS). The procedure has been validated in order to obtain the highest efficiency at the lowest concentration levels of analytes to fulfill the requirements of regulations on maximum residue limits. Under the optimum conditions, the linearity range was within 0.0096-100 μg L −1 . The limits of detection (LODs) of the developed DLLME-GC-MS methodology for all investigated pesticides were in the range of 0.0032 (endrin)-0.0174 (diazinon) μg L −1 and limits of quantification (LOQs) from 0.0096 to 0.052 μg L −1 . At lower concentration of 1 μg L −1 for each pesticide, recoveries ranged between 84% (tebufenpyrad) and 108% (deltamethrin) with relative standard deviations (RSDs) (n = 7) from 1.1% (metconazole) to 11% (parathion-mehtyl). This methodology was successfully applied to check contamination of environmental samples. The procedure has proved to be selective, sensitive and precise for the simultaneous determination of various pesticides. The optimized analytical method is very simple and rapid (less than 5 min).

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“…Gas chromatography (GC) with various detectors including flame ionization detector (FID) [13,14], electron capture (ECD) [15], nitrogen-phosphorus detection (NPD) [15,16], mass spectrometric detector (MS) [7,8,17], tandem mass spectrometry (MS/MS) [5], capillary liquid chromatography coupled with diode array detection (cHPLC-DAD) [3], ultra-high pressure liquid chromatography coupled to MS/MS (UHPLC-MS/MS) [4] and liquid chromatography with MS/MS (LC-MS/MS) [18] have been used for determination of pesticides residues in wine. UHPLC-MS/MS [4], GC-ECD, GC-MS [19] and LC-MS/MS [20] were reported for determination of pesticide residues in beer [20].…”

Section: Introductionmentioning

confidence: 99%

Salting-out Assisted Liquid-Liquid Extraction for the Determination of Multiresidue Pesticides in Alcoholic Beverages by High Performance Liquid Chromatography

Bedassa¹

2017

SJAC

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Abstract:A salting-out assisted liquid-liquid extraction (SALLE) method followed by high-performance liquid chromatography with ultraviolet-visible detector (HPLC-UV/Vis) has been proposed for determination of five multiclass pesticides residues including, atrazine, ametryn, terbutryn, carbaryl and chlorothalonil from various alcoholic beverages: beer, wine and Ethiopian honey wine (Tej). Experimental parameters influencing the extraction efficiency of the method such as the type and concentration of salt, volume of acetonitrile (the extraction solvent) and pH of the sample were assayed and the optimum conditions were established. Under the optimum experimental conditions, matrix-matched calibration curves were constructed using beer sample as the representative matrix and good linearity over wide concentration ranges were obtained with coefficient of determination (r 2 ) of 0.997 or better. The limits of detection (LOD) and quantification (LOQ) of the method, which were determined as 3 and 10 times a signal-to-noise ratio (S/N), were in the ranges of 1.3-3.9 and 4.5-12.8 µg L -1 , respectively. Precisions studied in terms of repeatability and intermediate precision (with-in lab reproducibility) at two concentration levels have demonstrated acceptable %RSD values, which were less than 10% in both cases. The applicability of the method was also investigated by analyzing various alcoholic beverages and demonstrated satisfactory recoveries in the ranges of 71-104% with their corresponding %RSDs less than 10% in all cases. The results of the study revealed that the developed SALLE method is selective and efficient sample preparation procedure prior to quantitative analysis of the target analytes by HPLC-UV/Vis.

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Ultrasound-vortex-assisted dispersive liquid–liquid microextraction coupled with gas chromatography with a nitrogen–phosphorus detector for simultaneous and rapid determination of organophosphorus pesticides and triazines in wine

Cited by 62 publications

References 44 publications

Ultrasound Vortex Assisted Dispersive Liquid-Liquid Microextraction (Usvadllme) Applied to the Determination of the Triazole Flutriafol and Triazines and Triazinones Pesticides in Water

Ultrasound Vortex Assisted Dispersive Liquid-Liquid Microextraction (Usvadllme) Applied to the Determination of the Triazole Flutriafol and Triazines and Triazinones Pesticides in Water

Fast, sensitive and reliable multi-residue method for routine determination of 34 pesticides from various chemical groups in water samples by using dispersive liquid–liquid microextraction coupled with gas chromatography–mass spectrometry

Salting-out Assisted Liquid-Liquid Extraction for the Determination of Multiresidue Pesticides in Alcoholic Beverages by High Performance Liquid Chromatography

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