Ultra-pressure liquid chromatography–electrospray tandem mass spectrometry for multiresidue determination of pesticides in water

Gervais, Gaël; Brosillon, Stéphan; Laplanche, A.; Helen, Céline

doi:10.1016/j.chroma.2008.07.006

Cited by 142 publications

(74 citation statements)

References 48 publications

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“…The most recent papers have reported methods using ultra-high-pressure liquid chromatography (UHPLC) coupled to MS/MS for ultra fast separations and sensitive determination of these compounds [26][27][28][29]. UHPLC provides higher peak capacity, greater resolution, increased sensitivity and high speed of analysis by the use of stationary phases of particle size (<2 m) smaller than conventional HPLC.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous determination of triazines and their main transformation products in surface and urban wastewater by ultra-high-pressure liquid chromatography–tandem mass spectrometry

et al. 2010

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This work describes the optimization, validation and application to real samples of an ultra-high-pressure liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method for the quantification and confirmation of 11 compounds (atrazine, simazine, terbuthylazine, terbumeton, terbutryn and their main transformation products) in surface and wastewater samples. Most of these analytes are included in the list of priority substances in the framework on European Water Policy. The application of this method to water samples reveals that the most relevant transformation products (TPs) should be incorporated into current analytical methods (which are focused mainly on the determination of unchanged compounds), to obtain a more realistic knowledge on water quality regarding pesticide contamination. TPs are generally more polar and mobile than the parents and they can be transported to the aquatic environment more rapidly than their precursors. Additionally, they can present some degree of toxicity and in fact TPs are also included within the legislation on drinking water as pesticide derivatives.To efficiently combine UHPLC with MS/MS, a fast-acquisition triple quadrupole mass analyzer was used.Working in selected reaction monitoring mode, up to three simultaneous transitions per compound were acquired allowing a reliable identification at ng/L levels. The method developed includes a pre-concentration step based on solid-phase extraction (OASIS HLB cartridges). Satisfactory recoveries (70-120%) and relative standard deviations (<20%) were obtained for all compounds in different water samples types spiked at two concentration levels (0.025 and 0.1 µg/L). The optimized method was found to have excellent sensitivity with instrumental detection limits as low as 50 fg.In addition, the influences of the matrix constituents on ionization efficiency and extraction recovery have been studied in different types of Italian and Spanish surface and urban wastewater. Signal suppressions were observed for all compounds, especially for influent wastewater. The use of isotope-labelled internal standards was found to be the best approach to assure an accurate quantification in all matrix samples.

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Section: Introductionmentioning

confidence: 99%

Simultaneous determination of triazines and their main transformation products in surface and urban wastewater by ultra-high-pressure liquid chromatography–tandem mass spectrometry

et al. 2010

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“…27 Several methods have been published multiresidues using detection by mass spectrometry. [28][29][30][31] However, nitrogen and phosphorus detector combined with an appropriate extraction method is also able to detect different classes of pesticides with high sensitivity. Our study aimed at comparing SPE and SPME extraction procedures for pre-concentration of selected pesticides from aqueous matrices in order to achieve the detection levels required by Brazilian legislation.…”

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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“…Recently, ultra high pressure liquid chromatography (UHPLC) has been developed as an innovative and powerful separation technique based on the use of stationary phases of particle size (<2 m) smaller than in conventional HPLC. UHPLC coupled to MS/MS has been shown as an excellent analytical tool for multi-class analysis of water for compounds like pharmaceuticals and drugs [16][17][18][19], toxins [20] or pesticides [21,22], due to its improved selectivity and sensitivity. With the modern QqQ analyzers even more than two SRM transitions can be acquired for a safe identification without losing sensitivity.…”

Section: Introductionmentioning

confidence: 99%

“…based on SPE) is typically required in multi-class methods where a large number of contaminants are determined [16][17][18][19][20][21][22].…”

Section: Introductionmentioning

confidence: 99%

Analytical strategy based on the use of liquid chromatography and gas chromatography with triple-quadrupole and time-of-flight MS analyzers for investigating organic contaminants in wastewater

et al. 2010

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The presence of a wide variety of organic pollutants with different physico-chemical characteristics has been investigated in wastewater samples from a municipal solid waste treatment plant placed at Castellón, Spain. An advanced analytical strategy has been applied, consisting on the combined used of two powerful and complementary techniques, GC and LC, both hyphenated with tandem mass spectrometry with triple quadrupole analyzers. The GC-MS/MS method was based on sample extraction using The most commonly detected pollutants were herbicides (simazine, terbuthylazine, terbutryn, terbumeton, terbacil and diuron), together with fungicides (thiabendazole and carbendazim) and 4-t-octylphenol. In the light of data obtained, it has been proven that reverse osmosis process used for water treatment was efficient and notably reduced the levels of organic contaminants found in raw leachate samples. 3In order to investigate the presence of other non-target contaminants, water samples were also analyzed by using GC-TOF MS and LC-QTOF MS. Several organic pollutants that did not form a part of the previous list of target contaminants were identified in the samples, thanks to the good sensitivity of TOF MS in full spectrum acquisition mode and the valuable accurate mass information provided by these instruments. The insecticide diazinon, the fungicide diphenylamide, the UV filter benzophenone, N-butyl benzenesulfonamide (N-BBSA), the insect repellent diethyltoluamide, caffeine or pharmaceuticals like erythromycin, benzenesulfonanilide, ibruprofen, atenolol or paracetamol, were some of the compounds identified in the water samples analyzed.

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Ultra-pressure liquid chromatography–electrospray tandem mass spectrometry for multiresidue determination of pesticides in water

Cited by 142 publications

References 48 publications

Simultaneous determination of triazines and their main transformation products in surface and urban wastewater by ultra-high-pressure liquid chromatography–tandem mass spectrometry

Simultaneous determination of triazines and their main transformation products in surface and urban wastewater by ultra-high-pressure liquid chromatography–tandem mass spectrometry

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

Analytical strategy based on the use of liquid chromatography and gas chromatography with triple-quadrupole and time-of-flight MS analyzers for investigating organic contaminants in wastewater

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