Azadirachtoids were determined by liquid chromatography/mass spectrometry (LC/MS) in five methanolic seed extracts of the neem tree and in a commercial formulation. On average, seed extracts contain azadirachtin A (10.9%), azadirachtin B (3.5%), nimbin (10.4%), and large quantities of salannin (19.0%). The composition of the commercial formulations may present different azadirachtoids contents depending on the natural extracts used in the preparation. Because these compounds may also show insecticide activity, the efficacy on field of these formulations may be very different. Photodegradation of pure azadirachtoids was also studied. Azadirachtins and related compounds are very sensitive to sunlight, degrading rapidly, with half-lives of the order of 11.3 h for azadirachtin A and 5.5 h for azadirachtin B and few minutes for the other limonoids compounds studied. The residues of azadirachtins and the main constituents, e.g., salannin, nimbin, deacetylnimbin, and deacetylsalannin, of the neem seed extract were determined on strawberries after field treatment using two different formulations. This residue study on strawberry was carried out to assess not only the azadirachtin content but also the main azadirachtoids contents. Three days after field application at five times the dose recommended by the manufacturer, residues of azadirachtin A and B were 0.03 and 0.01 mg/kg, respectively, while residues of salannin (LOQ 0.01 mg/kg) and nimbin (LOQ 0.5 mg/kg) were not detectable.
The behavior of pyrethrins and piperonyl butoxide (PB) on peaches has been studied after field treatment. Three experiments were carried out at 1, 5, and 10x the concentration recommended by the manufacturer. In all experiments, the initial deposition was below the maximum residue level (MRL), and the half-life time calculated in the 10x experiment for total pyrethrins within 2.3 days was in agreement with the preharvest interval (PHI) recommended. In a model system, the photodegradation rates of the pyrethrins in three commercial products were compared with pyrethrum pale (PP), with and without the presence of peach waxes. The pyrethrins in formulations containing PB showed higher half-life times but were not influenced by the presence of waxes, whereas in the case of PP that does not contain any PB, photodegradation was significantly affected by the presence of waxes.
Care should be taken when using pesticides in greenhouse conditions, because degradation mainly affects fruit growth. The size of the tomato, in particular its surface/weight ratio, is very important for defining pesticide residues. All fungicides used showed residue levels below the MRLs at the preharvest interval.
Bioconcentration factors (BCFs) were estimated for all congeners in each of the C(4) through C(8) homologue groups for perfluorinated alkylsulfonic acids (PFSAs) and alkylcarboxylic acids (PFCAs). Predictive equations were developed between molecular areas and volumes using optimized gas-phase geometries from the AM1 and PM3 semiempirical computational basis sets and previously determined BCFs for representative straight-chain members of each contaminant class. Molecular area approaches for estimating PFSA and PFCA BCFs resulted in more variability both between and within homologue groups than the use of molecular volumes as proxies for hydrophobicity of the perfluoroalkyl chain. An increasing degree of perfluoroalkyl chain branching within each homologue group reduces the estimated BCF, suggesting that the more linear PFSA and PFCA congeners will display the highest BCFs in aquatic organisms.
The behavior in field and the transfer from grapes to wine during winemaking of iprovalicarb, indoxacarb, and boscalid was studied. The residue levels found in grapes were far below the MRLs set for grapes in EU, accounting at harvest time 0.81, 0.43, and 4.23 mg/kg for iprovalicarb, indoxacarb, and boscalid, respectively. The residue levels in the samples treated with boscalid may have residual problems (due to an accumulation effect) if repeated field treatments will be performed. Winemaking experiments showed a complete transfer of all pesticide from grapes to the must, while in wine the residues were low or negligible due to the adsorbing effect of lees and pomace. The clarification experiments showed a good removal of pesticide residues from the wine media, for all pesticides. The GC-ITMS method showed good performance with adequate recoveries ranging from 75 to 115%, and good method limits of quantitation (LOQs) and of determination (LODs) far below MRLs.
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