Determination of pesticide residues in wine by membrane-assisted solvent extraction and high-performance liquid chromatography–tandem mass spectrometry

Abstract

The determination of pesticides in food products is an essential issue to guarantee food safety and minimise health risks of consumers. A protocol based on membrane-assisted solvent extraction and liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) that allows the determination of 18 pesticides in red wine at minimum labour effort for sample preparation was developed and validated. Ten millilitres of wine were extracted using 100 μL of toluene filled in a non-porous polyethylene membrane bag which is immersed in the wine sample. After 150 min extraction under stirring, an aliquot of the extraction solution is analysed using HPLC-MS/MS. The limits of quantification ranged from 3 ng/L for Pirimicarb to 1.33 μg/L for Imidacloprid. Quantification by matrix-matched calibration provided relative standard deviations ≤16 % for most of the target pesticides. The linearity of calibration was given over three to four orders of magnitude, which enables the reliable measurement of a broad range of pesticide concentrations, and for each target pesticide, the sensitivity of the protocol meets the maximum residue levels set by legislations at least for wine grapes. Good agreement of results was found when the new method was compared with a standard liquid-liquid extraction protocol. In five wine samples analysed, Carbendazim and Metalaxyl were determined at micrograms per litre concentrations, even in some of the organic wines. Tebuconazol and Cyprodinitril were determined at lower abundance and concentration, followed by Spiroxamin and Diuron.

Moiety and linker site heterologies for highly sensitive immunoanalysis of cyprodinil in fermented alcoholic drinks

“…Several methods have been described for the detection of cyprodinil traces in wines, based on gas or liquid chromatography with mass spectrometry detection. A previous extraction step is usually employed to avoid matrix effects, such as solid-phase microextraction with divinylbenzeneecarboxenepolydimethylsiloxane fibres (Rial-Otero, Yagüe-Ruiz, Cancho-Grande, & Simal-G andara, 2002), liquideliquid extraction (Vaquero-Fern andez et al, 2008), solid-phase extraction with Oasis HLB cartridges (Fontana, Rodríguez, Ramil, Altamirano, & Cela, 2011), dispersive liquideliquid microextraction (Rodríguez-Cabo, Rodríguez, Ramil, & Cela, 2011), or the QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure (Moeder, Bauer, Popp, van Pinxteren, & Reemtsma, 2012;Walorczyk, Drozdzynski, & Gnusowski, 2011). Also, immunoassays have been developed and validated in wines for the analysis of pesticides like benalaxyl (Rosso, Giraudi, Gamberini, Baggiani, & Vanni, 2000), tebufenozide (Irwin, Tolhurst, Jackson, & Gale, 2003), fenhexamid (Mercader & Abad-Fuentes, 2009), or bromopropylate (Ramon-Azc on, S anchez-Baeza, Sanvicens, & Marco, 2009), showing excellent performance.…”

Monoclonal antibody-based immunoassays for cyprodinil residue analysis in QuEChERS-based fruit extracts

“…These processing and measurement methods provide highly sensitive and robust analysis, and possess the capacity to determine simultaneously a variety of residues. Recently, several studies have been published describing chromatographic multiresidue analytical approaches comprising cyprodinil analysis in wine (Rial-Otero, Yagüe-Ruiz, Cancho-Grande, & Simal-Gándara, 2002;Vaquero-Fernández et al, 2008;Zhang et al, 2009;Fontana, Rodriguez, Ramil, Altamirano, & Cela, 2011;Moeder, Bauer, Popp, van Pinxteren, & Reemtsma, 2012), vegetable (Melo, Aguiar, Mansilha, Pinho, & Ferreira, 2012), and strawberry (Fernandes, Domingues, Mateus, & Delerue-Matos, 2012) samples. Additionally, contemporary analysts requiring sensitive, simple, rapid, specific, and high sample throughput approaches may recourse to molecular receptor-based techniques, like the competitive enzyme-linked immunosorbent assay (cELISA).…”

Ecological Risk Assessment of Soil Heavy Metals and Pesticide Residues in Tea Plantations

“…While its concentration might not have been detected or at low amount in the study sites, Das et al [32] report that such insecticides tend to reduce ammonifying and nitrifying bacteria and increase non-symbiotic N-fixing bacteria in the soil thus resulting in negative effects on total N and organic C. Bifenthrin is also a pyrethroid pesticide widely used in agriculture. Its half-life can be up to 345 d and has become an environmental concern [33]. Such issues should be considered, especially for sustainable tea plantations where soil management can be quite complex and site-specific.…”