Development of a liquid–liquid extraction method for the determination of pyrimethanil, metalaxyl, dichlofluanid and penconazol during the fermentative process of must by GC‐NPD

Vaquero-Fernández, Luis; Sanz-Asensio, Jesús; Fernández-Zurbano, Purificación; Sainz-Ramírez, Miguel; López-Alonso, Miguel; Epifanio-Fernández, Sara-Isabel; Martínez-Soria, María-Teresa

doi:10.1002/jsfa.3508

Cited by 11 publications

(9 citation statements)

References 24 publications

(29 reference statements)

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“…On the other hand, those micro‐organisms may play a role in the reduction of the amount of fungicide residues in the final wine. The decrease may be caused by degradation or adsorption/absorption . Various oenological practices carried out in the winemaking process, such as clarification and filtration, can produce a reduction in residues that remain after fermentation …”

Section: Introductionmentioning

confidence: 99%

“…A subsequent purification of the extracts is usually performed. Traditionally, sample preparation is carried out either by liquid–liquid extraction (LLE) using organic solvents or by solid phase extraction (SPE) using reverse phase materials . For the determination, chromatographic techniques are normally used.…”

Section: Introductionmentioning

confidence: 99%

“…For the determination, chromatographic techniques are normally used. Gas chromatography (GC) with nitrogen–phosphorus detection (NPD), electron capture detection (ECD) or mass spectrometry (MS) detection has been widely used . High‐performance liquid chromatography (HPLC) is the best choice when the compounds are thermally unstable or not volatile.…”

Section: Introductionmentioning

confidence: 99%

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Determination of fungicide pyrimethanil in grapes, must, fermenting must and wine

et al. 2012

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BACKGROUND This study determined the evolution of pyrimethanil, a fungicide commonly used to control Botrytis cinerea, throughout the winemaking process in grapes, must, fermenting must and wine. Tempranillo grapevines were treated with pyrimethanil according to both good Agricultural Practices (GAP) and Critical Agricultural Practices (CAP). Fermentation was carried out in an experimental winery. Grape analysis was based on an ethyl acetate extraction method. Samples from fermentation were analysed by solid phase extraction. The determination was carried out by gas chromatography with nitrogen–phosphorus detection (GC‐NPD) and additionally confirmed by gas chromatography/mass spectrometry (GC/MS). RESULTS Pyrimethanil residues were at least ten times greater in grapes treated 7 days before harvest than in those treated respecting the safety period (21 days). The amount of pyrimethanil in grapes treated under GAP was below the maximum residue limit (5 mg kg−1). The level of pyrimethanil decreased during fermentation in both treatments. In the fermentation of grapes treated according to CAP, the pyrimethanil concentration was reduced by over 50% on the first day and then remained constant until the end of the fermentation process. For grapes treated in compliance with GAP, the amount of pyrimethanil decreased to a level below the limit of detection in the bottled wine. CONCLUSION The described methods for grapes, must, fermenting must and wine gave good recoveries, linearity, precision and accuracy. They were also highly sensitive in avoiding matrix effects. Pyrimethanil residues found in treated grapes were higher in skin than in pulp. The amount of pyrimethanil decreased during fermentation by degradation and/or adsorption. For grapes treated according to GAP, residues disappeared in the final bottled wine. The decrease observed in the final bottled wine may be caused by diverse oenological practices and technologies such us malolactic fermentation, racking and settling. © 2012 Society of Chemical Industry

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Determination of fungicide pyrimethanil in grapes, must, fermenting must and wine

et al. 2012

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“…The calibration was checked routinely. Limits of detection (LOD) and quantification (LOQ) were determined by injecting standard solution (n = 6) and measuring background response (noise) [18]. Results showed that the LODs of all 18 OPPs were below the MRLs.…”

Section: Calibration Curves Limits Of Detection and Quantificationmentioning

confidence: 99%

One-step extraction for gas chromatography with flame photometric detection of 18 organophosphorus pesticides in Chinese medicine health wines

Liu

Kong

Qiu

et al. 2012

Journal of Chromatography B

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“…[5][6][7][8][9][10] Fungicide residues in wine are usually analyzed by chromatographic multianalyte methods, particularly highperformance liquid chromatography with mass spectrometry detection (HPLC-MS), supported by sample extraction procedures like QuEChERS (acronym for Quick, Easy, Cheap, Effective, Rugged, and Safe). [11][12][13] Moreover, alternative extraction methodologies have also been developed recently for the analysis of anilinopyrimidine residues in wine using liquid-liquid extraction, 14 solid-phase extraction, 15,8,16 solidphase microextraction, 17 dispersive liquid-liquid microextraction, 7 bar adsorptive microextraction, 18 and ultrasound-assisted microextraction. 19,20 Adoption of bioanalytical techniques for the determination of chemical residues and contaminants has been increasing during the last decades, being the competitive enzyme-linked immunosorbent assay (ELISA) one of the most extended immunochemical methods because of a series of great advantages like simplicity, high sensitivity, portability, affordable cost, and high sample throughput.…”

Section: Introductionmentioning

confidence: 99%

A class-selective immunoassay for simultaneous analysis of anilinopyrimidine fungicides using a rationally designed hapten

Esteve‐Turrillas

Mercader

Agulló

et al. 2017

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The development of multianalyte immunoassays constitutes a main research issue in the field of bioanalytical techniques. In the present study, class-specific antibodies against the three members of the anilinopyrimidine family of fungicides (pyrimethanil, cyprodinil, and mepanipyrim) were raised by using a bioconjugate of a rationally designed hapten [5-(6-methyl-2-(phenylamino)pyrimidin-4-yl)pentanoic acid]. Highly sensitive immunoassays were developed for the generic determination of these compounds, using the competitive enzyme-linked immunosorbent assay (ELISA). Particularly, a direct antibody-coated competitive ELISA afforded identical sensitivity for the three anilinopyrimidines, with IC50 values of 0.26, 0.27, and 0.25 μg L −1 for pyrimethanil, cyprodinil, and mepanipyrim, respectively. This immunoassay was fully characterized and applied to the multianalyte determination of anilinopyrimidine fungicides in white and red wines, with a limit of quantification of 1 μg L −1, average recoveries from 93.1% to 114.4%, and relative standard deviations lower than 20%. Commercial wine samples were analyzed and those containing detectable anilinopyrimide residues were verified by a reference chromatographic technique.

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Development of a liquid–liquid extraction method for the determination of pyrimethanil, metalaxyl, dichlofluanid and penconazol during the fermentative process of must by GC‐NPD

Cited by 11 publications

References 24 publications

Determination of fungicide pyrimethanil in grapes, must, fermenting must and wine

Determination of fungicide pyrimethanil in grapes, must, fermenting must and wine

One-step extraction for gas chromatography with flame photometric detection of 18 organophosphorus pesticides in Chinese medicine health wines

A class-selective immunoassay for simultaneous analysis of anilinopyrimidine fungicides using a rationally designed hapten

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