Validation and uncertainty study of a comprehensive list of 160 pesticide residues in multi-class vegetables by liquid chromatography–tandem mass spectrometry

Kmellár, Béla; Fodor, Péter; Pareja, Lucía; Ferrer, Carmen María Salvador; Martínez‐Uroz, M. A.; Valverde, Antonio; Fernández‐Alba, Amadeo R.

doi:10.1016/j.chroma.2008.10.121

Cited by 296 publications

(170 citation statements)

References 17 publications

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“…The original procedure consists of extracting the homogenized sample by hand-shake or Vortex with the same amount of acetonitrile in order to have a final extract concentrated enough without the need of a solvent evaporation step. The technique has attracted the attention of pesticide analysis studies worldwide, [15][16][17][18] and a review has been published recently. 19 In the other hand, the research about pesticides analysis in dry samples (e.g.…”

Section: Introductionmentioning

confidence: 99%

A new gas chromatography/mass spectrometry (GC-MS) method for the multiresidue analysis of pesticides in bread

Kolberg¹,

Prestes²,

Adaime³

et al. 2010

J. Braz. Chem. Soc.

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Neste trabalho desenvolveu-se um método para a determinação de 15 pesticidas em pão utilizando cromatografia gasosa acoplada à espectrometria de massas (GC-MS), operando no modo de ionização química negativa (NCI). No preparo da amostra utilizou-se acetonitrila contendo 1% (v/v) de ácido acético, na presença de acetato de sódio, citrato de sódio e sulfato de magnésio. O método foi validado avaliando os seguintes parâmetros: linearidade, limite de detecção (LOD), limite de quantificação (LOQ), precisão e exatidão. A faixa linear utilizada foi de 1,0-100 µg L -1 . As recuperações foram consideradas satisfatórias apresentando valores entre 70 e 117%, com RSD ≤ 17,6% para quase todos os compostos. O LOQ do método variou de 10 a 20 µg kg -1 . O método demonstrou ser adequado, sensível e altamente seletivo para a análise multirresíduo de pesticidas em pão.In this work a method for the determination of 15 pesticides in bread samples using gas chromatography coupled with mass spectrometry (GC-MS), operating in the negative chemical ionization mode (NCI) was developed and validated. For the extraction procedure acetonitrile containing 1% (v/v) acetic acid was used in presence of sodium acetate, sodium citrate and magnesium sulphate. The method was validated evaluating the following parameters: linearity, limit of detection (LOD), limit of quantification (LOQ), precision and accuracy. The linear range used was from 1.0 to 100 µg L -1 . The recoveries had been considered satisfactory presenting values between 70 and 117% with RSD ≤ 17.6% for almost all the compounds. The real method LOQ ranged from 10 to 20 mg kg -1 . The method shown to be adequate for the multiresidue analysis of pesticides in bread and the GC-MS (NCI) proved to be sensitive and highly selective.

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Section: Introductionmentioning

confidence: 99%

A new gas chromatography/mass spectrometry (GC-MS) method for the multiresidue analysis of pesticides in bread

Kolberg¹,

Prestes²,

Adaime³

et al. 2010

J. Braz. Chem. Soc.

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“…It was considered to be a mild signal suppression or enhancement effect of between -20 and +20%. The values of these 11 kinds of organophosphorus pesticides were between 92 and 96% for each target analyte, 28 and the clean-up procedure performed well.…”

Section: Matrix Effectsmentioning

confidence: 93%

Determination of Eleven Organophosphorus Pesticide Residues in Textiles by Using HPLC-HRMS

et al. 2017

ANAL. SCI.

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“…17 They usually include a liquid-liquid extraction (LLE), 18,28 solid-phase extraction (SPE), 19,22,[41][42][43] solid-phase microextraction (SPME), 44,45 matrix solid-phase dispersion (MSPD), [46][47][48] liquid-liquid microextraction, 49 dispersive liquid-liquid microextraction (DLLME), 50,51 temperature controlled ionic liquid dispersive liquid phase microextraction, 52 carbon nanotube reinforced hollow fiber liquid-phase microextraction 53 or supercritical fluid extraction 54 followed by gas 20,50,[55][56][57][58][59][60] or liquid chromatography. 1,19,48,49,52,53,[61][62][63][64][65][66][67][68][69][70] The low volatility and the thermolability of these compounds and the high polarities of the transformation products obviously favor the use of column liquid chromatography (LC) as the separation technique.…”

Section: Introductionmentioning

confidence: 99%

“…17,[30][31][32] The identification of these compounds in different matrices as well as their quantification are of interest in the criminal field since the number of human 3,17,[33][34][35][36] 53 or supercritical fluid extraction 54 followed by gas 20,50,[55][56][57][58][59][60] or liquid chromatography. 1,19,48,49,52,53,[61][62][63][64][65][66][67][68][69][70] The low volatility and the thermolability of these compounds and the high polarities of the transformation products obviously favor the use of column liquid chromatography (LC) as the separation technique.Due to the low detection levels required by regulatory agencies, efficient sample preparation and trace-level detection are important aspects in an analytical method. The extraction and cleanup steps are sometimes carried out simultaneously using techniques such as solid-phase extraction (SPE) and solvent extraction with low temperature partitioning (SE-LTP).…”

mentioning

confidence: 99%

Determination of carbamates in beverages by liquid-liquid extraction with low temperature partitioning and liquid chromatography

Goulart¹,

Alves²,

Paula³

et al. 2012

J. Braz. Chem. Soc.

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Carbamatos são os pesticidas mais frequentemente encontrados em alimentos e bebidas de coloração escura em casos de intoxicação acidental ou intencional. Neste trabalho, extração líquido-líquido com partição em baixa temperatura (LLE-LTP) foi otimizada e validada para determinação dos carbamatos aldicarb, carbofuran e carbaril em bebidas de sucos de uva e leite achocolatado. Este método envolve a extração com acetonitrila, partição líquido-líquido em baixa temperatura e análise por cromatografia líquida de alta eficiência com detecção ultravioleta (HPLC-UV). O método é rápido, eficiente e de baixo custo, emprega pequenos volumes de solvente por amostra e não necessita de limpeza dos extratos. O método de extração foi seletivo e apresentou porcentagens de extração acima de 90%. As premissas relacionadas com os testes estatísticos de linearidade foram verificadas e confirmadas. O método de extração e análise foi validado com resultados satisfatórios e pode ser aplicado em análises de rotina e forenses.Carbamates are the pesticides most commonly found in dark colored foods and beverages in cases of accidental or intentional poisoning. In this work, the liquid-liquid extraction with low temperature partitioning (LLE-LTP) was optimized and validated for determination of the carbamates aldicarb, carbofuran and carbaryl in grape juice and chocolate milk beverages. This method involved extraction with acetonitrile, liquid-liquid partition at low temperature and the analysis by high performance liquid chromatography with ultraviolet detection (HPLC-UV). The method is rapid, efficient and of low-cost, employing small volumes of solvent per sample and requiring no cleanup of the extracts. The extraction methodology was selective and presented recovery percentages above 90%. The premises related to the statistical linearity tests were checked and confirmed. The method of extraction and analysis was validated with satisfactory results, and may be applied in forensic and routine analysis Keywords: carbamates, low temperature partitioning, high performance liquid chromatography, sample preparation, validation IntroductionCarbamate insecticides are widely used in gardening and agriculture due to their broad spectrum of activity and relatively short environmental persistence. However, they are potentially toxic to humans, particularly in the context of intentional self-poisoning. 1,2 Carbamates are found as commercialized products for agricultural practices and some compounds of this group, with their respective commercial names are: carbaryl (Sevin ® ), aldicarb (Temik ® ) and carbofuran (Furadan ® ). From these, aldicarb stands out as the main target on the list of controlled pesticides of the United States Environmental Protection Agency (EPA) due to its elevated toxicity to mammals. 3,4 The maximum residue level (MRL) of aldicarb 5,6 and carbofuran 6 in water is 10 and 7 μg L -1 , respectively. In Goulart et al. 1155 Vol. 23, No. 6, 2012 milk, the MRLs established for aldicarb, 7,8 Exposures may occur accidentally, with ...

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Validation and uncertainty study of a comprehensive list of 160 pesticide residues in multi-class vegetables by liquid chromatography–tandem mass spectrometry

Cited by 296 publications

References 17 publications

A new gas chromatography/mass spectrometry (GC-MS) method for the multiresidue analysis of pesticides in bread

A new gas chromatography/mass spectrometry (GC-MS) method for the multiresidue analysis of pesticides in bread

Determination of Eleven Organophosphorus Pesticide Residues in Textiles by Using HPLC-HRMS

Determination of carbamates in beverages by liquid-liquid extraction with low temperature partitioning and liquid chromatography

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