Optimization of a matrix solid-phase dispersion method with subsequent clean-up for the determination of ethylene bisdithiocarbamate residues in almond samples

Martínez, Rosa María Goig; Ramos, Lourdes; Fernández-Hernando, P.; Cámara, Carmen

doi:10.1016/j.chroma.2004.04.043

Cited by 42 publications

(4 citation statements)

References 25 publications

(25 reference statements)

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“…This technique combines both sample homogenization and a possible preliminary clean-up of the compounds of interest [21]. An advantage of this procedure is that no emulsion is formed [22], once the material is blended with a dispersion agent.…”

Section: Introductionmentioning

confidence: 99%

p‐Nitro‐N‐propylaniline/silica: Synthesis, characterization, and its application in matrix solid phase dispersion for multiresidue analysis of pesticides in carrots

Abad

Winck

Benvenutti

et al. 2007

J of Separation Science

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A new material for matrix solid phase dispersion (MSPD) was synthesized -- p-nitro-N-propylaniline/silica (pNNPASi) by grafting reactions, characterized by elemental analysis and N(2)-adsorption-desorption isotherms, and tested for multiclass multiresidue analysis of pesticides in wet and freeze-dried carrots. Results obtained applying this new solid phase sorbent to MSPD extraction of ten pesticides (trichlorphon, trifluralin, dicloran, chlorothalonil, prometryn, linuron, captan, procymidone, prochloraz, and deltametrin) in wet carrots showed better results than the ones obtained for freeze-dried samples. Recoveries were in the range of 48-106% and precisions varied from 6 to 20% when wet samples were employed. Comparison between pNNPASi sorbent and C(18) showed better performance of pNNPASi for eight out of ten pesticides tested. The LOQs show that the developed method can be used to detect the pesticides investigated in carrots at concentrations below the maximum residue levels (MRL) established by EU, USEPA, and National Sanitary Surveillance Agency (ANVISA). Linuron, captan, prochloraz, and deltamethrin were found in at least one of the two commercial samples studied in concentrations above the LOQ of this method. Concentrations of the last three pesticides were above the European MRL in one of the commercial samples.

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Section: Introductionmentioning

confidence: 99%

p‐Nitro‐N‐propylaniline/silica: Synthesis, characterization, and its application in matrix solid phase dispersion for multiresidue analysis of pesticides in carrots

Abad

Winck

Benvenutti

et al. 2007

J of Separation Science

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“…Garcinun ˜o et al have used MSPD to extract carbamate residues from almond samples with a subsequent cleanup step by SPE using alumina and C-18 as the sorbent, but the results were unsatisfactory because large amounts of fat were present. To overcome this problem, the sample was first defatted by alkaline hydrolysis with NaOH (7). Husain and co-workers analyzed diazinon and ethion in pistachio nuts by using MSPD and thin-layer chromatography (TLC) to separate pesticides from the pistachio extract followed by GC with nitrogen-phosphorus detection (NPD) (8).…”

Section: Introductionmentioning

confidence: 99%

Analysis of Pesticides in Nuts by Online Reversed-Phase Liquid Chromatography−Gas Chromatography Using the Through-Oven Transfer Adsorption/Desorption Interface

Cortés

Toledano

Villén

et al. 2008

J. Agric. Food Chem.

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A new method to determine pesticide residues in nuts is presented, in which the pesticides are extracted from samples with a small amount of ethyl acetate and anhydrous sodium sulfate. No additional cleanup or concentration steps are necessary. The extract is directly injected into the high-pressure liquid chromatograph, where preseparation of the pesticide residues from other components coextracted from the nuts is carried out using methanol/water as the eluent. The selected liquid chromatography fraction containing the pesticides is automatically transferred to the gas chromatograph using the through-oven transfer adsorption/desorption interface. The calculated limits of detection for each pesticide varied from 0.1 to 61.3 microg/kg. The repeatabilities of the analysis and the overall procedure (extraction and analysis) were satisfactory. No variations in the retention time were observed. The method was applied to the analysis of pistachio nut, peanut, walnut, hazelnut, and sunflower seed.

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“…MSPD combines both sample homogenization and a possible preliminary clean-up of the target compounds. 17,18 Advantages of this procedure are that no emulsion is formed and elution of the analytes is performed with a relative small solvent volume. 19 This technique also enhances the availability of the analytes as it promotes the disruption of the gross architecture of the sample.…”

mentioning

confidence: 99%

Multiresidue determination of pesticides in carrots using pressurized liquid extraction and gas chromatography with mass spectrometry detector

Abad¹,

Winck²,

Silva³

et al. 2010

J. Braz. Chem. Soc.

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Neste estudo, 14 agrotóxicos (captan, clorotalonil, deltametrina, dicloran, fention, folpete, iprodiona, linurom, malationa, prometrina, procloraz, procimidona, triclorfom e trifluralina) foram usados no desenvolvimento de um método multiresíduos (MRM), utilizando extração de cenouras com líquido pressurizado (PLE). A etapa de clean-up foi realizada por dispersão da matriz em fase sólida (MSPD), sendo testados como material dispersante o Florisil, XAD-4, XAD-7 e C18. Diclorometano, acetato de etila e acetona foram empregados como solventes para PLE, a 75 ºC e 1.500 psi. As recuperações dos analitos para cenouras liofilizadas ficaram na faixa de 70 a 133%. Entretanto, os percentuais de recuperação obtidos para as cenouras úmidas não foram satisfatórios (< 70%). Os coeficientes de determinação das curvas analíticas situaram-se na faixa de 0,9821 a 0,9997; os limites de detecção (LOD) e de quantificação (LOQ) para os vários compostos investigados ficaram entre 0,0024-0,1968 mg kg -1 e entre 0,0072-0,5963 mg kg -1 , respectivamente.In this study, 14 pesticides (captan, chlorothalonil, deltamethrin, dicloran, fenthion, folpet, iprodione, linuron, malathion, prometryn, prochloraz, procymidone, trichlorphon and trifluralin) were employed for developing a multiresidue method (MRM) using pressurized liquid extraction (PLE). In situ clean-up was achieved using matrix solid phase dispersion (MSPD), where Florisil, XAD-4, XAD-7 and C18 were tested as dispersing material for carrot samples. Dichloromethane, ethyl acetate and acetone were used as solvents in a PLE unit at 75 ºC and 1,500 psi. Recovery was in the range of 70 to 133 %. Results obtained with wet carrots were not satisfactory, since most of the recovery values were below 70%. Determination coefficients of the analytical curves presented values between 0.9821 and 0.9970. Limits of detection (LOD) and quantification (LOQ) for the various components varied from 0.0024 to 0.1968 mg kg -1 , and 0.0072 to 0.5963 mg kg -1 , respectively. Keywords: multiresidue method, PLE, MSPD, carrots, GC/MS IntroductionIn the last few decades, pesticides have been used on an increasingly wider scale throughout the world. On account of the large number of active ingredients used in agricultural production, complex analytical procedures are required for the detection of a great number of possible compounds, with few number of extraction and clean-up steps. These compounds are characterized by their diversity, their different physical and chemical properties (polarity, solubility, pKa etc) and their low concentrations in real samples. 1 Some of the analytical methods aim to determine a single component (SRM) and others, more sophisticated, are capable of simultaneously determine more than one residue in a single analysis. These last ones are called pesticide multiresidue methods (MRM) and comprise a higher degree of analytical difficulty. Multiresidue methodology by definition requires determinative steps for separating analytes from one another so each one can be detected and measured ...

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Optimization of a matrix solid-phase dispersion method with subsequent clean-up for the determination of ethylene bisdithiocarbamate residues in almond samples

Cited by 42 publications

References 25 publications

p‐Nitro‐N‐propylaniline/silica: Synthesis, characterization, and its application in matrix solid phase dispersion for multiresidue analysis of pesticides in carrots

p‐Nitro‐N‐propylaniline/silica: Synthesis, characterization, and its application in matrix solid phase dispersion for multiresidue analysis of pesticides in carrots

Analysis of Pesticides in Nuts by Online Reversed-Phase Liquid Chromatography−Gas Chromatography Using the Through-Oven Transfer Adsorption/Desorption Interface

Multiresidue determination of pesticides in carrots using pressurized liquid extraction and gas chromatography with mass spectrometry detector

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