The aim of this study was to compare pesticide residues, copper and biogenic amines concentrations in conventional and organic wines. For each type of wine production, 20 samples were collected. We ...used two multi-residual methods employing GC/MS (92 pesticides) and LC/MS/MS (112 pesticides) detection. Copper residues and biogenic amines were measured by standard FAAS and HPLC methods. We confirmed lower numbers and concentrations of pesticide residues in organic wines. The most frequently determined pesticide was dimethomorph, followed by boscalid, fenhexamid, metalaxyl + metalaxyl-M, iprovalicarb and pyrimethanil. Also, higher levels of copper were observed in the groups of conventional wines. For biogenic amines, we could not confirm a clear trend. It is unacceptable that some pesticide residues in organic wines were detected, which are not allowed in this type of production. Nevertheless, we can confirm the trend of added value in organic wine production in terms of reducing pesticide residues and copper in bottled wines.
-Added value is in organic wine production in terms of pesticides and copper reduction.-Producers should avoid some commonly found pesticide residues in the last sprays.-No significant difference in the occurrence and concentrations of biogenic amines between both groups of wines.
New analytical methods for the determination of pesticide residues in wine were introduced and validated. Extraction was performed with sorption of the active substances on the stir bar and ...determination by gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry. The methods were applied in practice. A total of 77 active substances were searched for in 42 wine samples from all 3 wine-growing regions of Slovenia. The fungicides dimethomorph, fludioxonil and pyraclostrobin were found in 78.6% of all analysed samples. The risk assessment concluded that the analysed wine samples do not pose an unacceptable risk to consumers. The results were compared with previous studies.
Pesticide residues in vinification process of two white and two red grapevine varieties were monitored during the 2007 vintage. Crushed grapes, cake, must, lees and wine were sampled during the ...vinification process. Additionally, grapes were sampled during the ripening process. All samples were taken in triplicate and analyzed for the presence of 117 pesticides. The pesticide residues were determined by three validated internal analytical methods: the multi-residual GC-MS method (71 pesticides), the multi-residual LC-MS-MS method (45 pesticides) and GC-MS method for the determination of dithiocarbamates (the sum of their concentrations is given as a concentration of carbon disulfide). Boscalid and phosalone were the most persistent pesticides in grapes during ripening. The concentrations of pesticide residues in must and wine were significantly diminished through separations during the solid and liquid phases of the vinification process, particularly the pressing of crushed grapes and wine racking after alcoholic fermentation. The pesticides detected throughout the vinification process were boscalid, cyprodinil, dimethomorph, fenhexamid, metalaxyl and procymidone and their concentrations in the wines were 0.01–0.02, 0.04, 0.01–0.08, 0.12–0.13, 0.09–0.11 and 0.07–0.13
mg
L
−1 respectively.
The capability of near infrared (NIR) spectroscopy was examined for the purposes of quality control of the traditional Slovenian dry-cured ham “
Kraški pršut.” Predictive models were developed for ...moisture, salt, protein, non-protein nitrogen, intramuscular fat and free amino acids in
biceps femoris muscle (n
=
135). The models' quality was assessed using statistical parameters: coefficient of determination (R
2) and standard error (se) of cross-validation (CV) and external validation (EV). Residual predictive deviation (RPD) was also assessed. Best results were obtained for salt content and salt percentage in moisture/dry matter (R
CV
2
>
0.90, RPD
>
3.0), it was satisfactory for moisture, non-protein nitrogen, intramuscular fat and total free amino acids (R
CV
2
=
0.75–0.90, RPD
=
2.0–3.0), while not so for protein content and proteolysis index (R
CV
2
=
0.65–0.75, RPD
<
2.0). Calibrations for individual free amino acids yielded R
CV
2 from 0.40 to 0.90 and RPD from 1.3 to 2.9. Additional external validation of models on independent samples yielded comparable results. Based on the results, NIR spectroscopy can replace chemical methods in quality control of dry-cured ham.
In the study we determined the pesticide residues and microbiological quality of bottled wines. Pesticide residues in wine were analysed using the multiresidual method with GC–MS, the multiresidual ...method with LC–MS–MS and the method for determination of dithiocarbamate residues with GC–MS. Furthermore, the effect of bentonite and the combined fining agent on the concentration of boscalid in wine was tested. The microbiological analysis was performed using membrane filtration. Nine pesticide residues were determined in the samples. More than 50% of wines belonged to the category of wines with only up to two pesticide residues. The most frequently determined pesticide in wines was boscalid (76% of samples) followed by fenhexamid (44%). The highest concentrations of pesticide residues in wines were determined for cyprodinil (0.44
mg/L) and fludioxonil (0.21
mg/L). The combined fining agent was more efficient in lowering the concentration of boscalid in wine if compared with bentonite. The results of microbiological quality indicate that no less than one quarter of bottled wines on our store shelves is microbiologically unstable.
In the period from 2005 to 2009 225 samples of apples, lettuce and potatoes from Slovene producers included in integrated pest management (IPM) were analysed for plant protection product (PPP) ...residues. The samples were analysed for the presence of more than 200 different active compounds using four analytical methods. In 38.7% of apple samples residues were not detected, 58.6% of apple samples contained residues lower than or equal to Maximum Residue Levels (MRLs) while 2.7% of apple samples exceeded MRLs. In 84.6% of lettuce samples residues were not detected, 12.3% of lettuce samples contained residues lower than or equal to MRLs while 3.1% of lettuce samples exceeded MRLs. In 98.0% of potato samples residues were not detected, 2.0% of potato samples contained residues lower than or equal to MRLs and no potato samples exceeded MRLs. Multiple residues were found only in apples and lettuce. The trend observed during the years was the decrease of sample portion of samples containing multiple residues in apples from 2005 to 2008. The most frequently found active substance in apples and lettuce was dithiocarbamates. In potato only phosalone was found.
Four analytical methods were developed and validated for the determination of veterinary drug residues and environmental pesticide residues in honey: (a) GC-MS method for the analysis of amitraz and ...all metabolites containing the 2,4-dimethylaniline moiety; (b) GC-MS method for the analysis of thymol, chlorfenvinphos and coumaphos; (c) GC-MS method for the analysis of 75 active substances; (d) LC-MS/MS method for the analysis of 60 active substances. Between the GC-MS (method c) and the LC-MS/MS method (method d) there was no overlap among active substances, meaning that using both methods 135 active substances originating from the environment in total were included and validated. The first method involved hydrolysis of amitraz and its metabolites containing the 2,4-dimethylaniline moiety to 2,4-dimethylaniline and extraction of 2,4-dimethylaniline to n-hexane. The other three methods had the same extraction procedure with a mixture of solvents: acetone, dichloromethane and petroleum ether. All 4 methods were tested in practice. Sixty samples of honey were analysed: 22 from organic and 38 from conventional production. Overall, residues were mainly higher than reported in literature but did not exceed MRLs. Risk assessment confirmed that the analysed samples are of no cause for concern for consumers.
Common buckwheat (Fagopyrum esculentum Moench) and tartary buckwheat (Fagopyrum tataricum Gaerth.) are underutilized pseudo-cereals and both considered nutritional food. Eight common and eleven ...tartary buckwheat accessions acquired from Slovenian plant gene bank were grown at the experimental fields of the Agricultural Institute of Slovenia in 2014. Dried grains were homogenised and analysed for several nutrient parameters: moisture content (11–14% dry weight, DW), total proteins (11–16 % DW), dietary fibre (15–19 % DW), ash (2–6 % DW) and total fats (1.8–2.6 % DW). The fatty acids (C14:0, C16:0, C18:0, C18:1n9, C18:2n6, C18:3n3, C20:0) were determined using gas chromatography, free amino acids (Gly, Glu, Arg, Lys, Asp, Ser, Phe, Ala, Val, Thr, Pro, Ile, Met, His, Cys, Leu, Tyr) by the high-performance liquid chromatography and multi-mineral analysis (K, P, Si, S, Ca, Fe, Cl, Ti, Zn) using X-ray fluorescence spectroscopy. The results show significant differences between two buckwheat species, and their gene bank accessions for investigated nutritional parameters.
Varietal thiol precursors in grapes are subject to metabolic changes during post-harvest treatments. Metabolic activity should therefore be limited after sampling to understand their biosynthesis in ...the berry and genetic regulation. In this study, berries were frozen in liquid nitrogen immediately after harvesting, transported in dry ice, stored briefly at -80 °C, cryo-milled and extracted without being thawed in cold methanol in a ratio of 1:4 (w/v). A UHPLC-MS/MS method for quantitative determination of the thiol precursors 3-S-glutathionylhexan-1-ol (G3MH), 3-S-cysteinylhexan-1-ol (Cys3MH), 4-S-glutathionyl-4-methylpentan-2-one (G4MMP) and 4-S-cysteinyl-4-methylpentan-2-one (Cys4MMP), glutathione, oxidized glutathione and L-methionine in grapes was developed. Reference material was provided through synthesis of precursors and their deuterium labelled analogues. The average thiol precursor content in grapes in 2013-15 was in the range 8-16 μg kg
for G3MH, 1-6 μg kg
for Cys3MH, 1-4 μg kg
for Cys4MMP and 0.3 μg kg
for G4MMP. In 2013 and 2014, the highest precursor content in mature Sauvignon Blanc grapes from vineyards located in Italy regarded G3MH, followed by Cys3MH, Cys4MMP and G4MMP. In 2015, G3MH was again the most abundant precursor, but followed by Cys4MMP, Cys3MH and G4MMP.
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