Journal of Food Science and Engineering 9 (2019) 81-87
doi: 10.17265/2159-5828/2019.03.001
Fate of Myclobutanil Residues after Application on Apples Growing to Korça District, Albania
Edlira Shahinasi1, Vojislava Bursic2, Martina Mezei2, Ferdi Brahushi3, Magdalena Cara4 and Gorica Vukovic5小屁孩日记下载
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1. Department of Chemistry, Faculty of Biotechnology and Food, Agricultural University of Tirana, Tirana 1029, Albania
2. Department of Environment and Plant Protection, Faculty of Agriculture, University of Novi Sad, Novi Sad 21000, Serbia
3. Department of Agro-environment and Ecology, Faculty of Agriculture, Agricultural University of Tirana, Tirana 1029, Albania
4. Department of Plant Protection, Faculty of Agriculture, Agricultural University of Tirana, Tirana 1000, Albania
5. Institute of Public Health, Belgrade 112113, Serbia
Abstract:One of the largest and most important pesticides groups are Demthylation inhibitors, a class of single-side fungicides, ud for the control of fungal dias on fruit. The aim of this study was to investigate the fate of myclobutanil after its application in Starking and Golden Delicious cultivars. The apple trees were treated with maximum and minimum levels of recommended dos. The samples were collected randomly in different interval days after application. For identification and quantification of myclobutanil residues in apple fruit liquid chromatography-tandem mass spectrometry (LC-MS/MS) technique was performed. The highest values of myclobutanil residues were found at the 1st day after treatment and by the time the residue levels were decread. Thus, the level of myclobutanil residues ranges from 0.928 mg kg-1 to 0.019 mg kg-1 and from 2.085 mg kg-1 to 0.086 mg kg-1 in Starking treated with the minimum and maximum dos respectively. Also, in the Golden Delicious cultivar the level of myclobutanil residues ranges from 0.878 mg kg-1 to 0.026 mg kg-1 and from 1.760 mg kg-1 to 0.092 mg kg-1 with the minimum and maximum applied dos at 1st and 40th day after application, respectively. Therefore, the samples treated with maximum recommended do did not reach the MRL (0.6 mg kg-1) before the 14th day after application, whereas the samples treated with minimum recommended do reached MRL before 7t
keepaliveh day after application. Therefore, the application of myclobutanil guarantees food safety for the consumer not only in minimum dos but even in maximal dos as well.
Key words: Apple, application dos, LC-MS/MS, myclobutanil, Korça district.
1. Introduction
The consumption of fruits and vegetables takes the cond place on the food pyramid of many European countries, after the cearls.
Fruits and vegetables are considered good sources in fibers, vitamins, minerals in the form of electrolytes and antioxidants [1-3]. According to World Health Organization (WHO) [2] a diet rich in fruits and vegetables may reduce the risk of heart dia, prevent some type of cancer, promote weight loss by reducing the risk of obesity at the same time.
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Among many fruit trees, apples are the most cultivated trees in Albania and the district of Korca
Corresponding author:Edlira Shahinasi M.Sc., rearch fields: environmental contaminants and food safety. reprents the main market suplier in the country. It occupied around 70% of total area planted with fruits and 83% of total fruit production [4, 5].
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Besides nutrient value and health benefits that fruits and vegetables posss, they can be sources of toxic substances if extensive pesticides are ud during the control of plant dias [3].
Among the most effective pesticides are the azoles or conazole, which are widely ud for controlling of apple dias. This group of fungicides belongs to demethylation inhibiter (DMI) fungicides which have a wide spectrum of activity [6].
Becau this class of fungicides is ud incrreasingly in many countries all over the world it is important to evaluate the fate of DMIs fungicides in fruits and environment [7]. The aim of this study was to
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Fate of Myclobutanil Residues after Application on Apples Growing to Korça District, Albania 82
determine prence of pesticide residues in apples and to asss if the fruits are safe for the consumers.
come up2. Materials and Methods
2.1 Experimental Field and Sampling
The experiment was conducted in Korça region as the main area of apple cultivation of apple in Albania, during 2015 and 2016. The experimental field was divided in four plots where two pots reprented Golden Delicious apple trees and two others reprented Starking apple trees. The pots were treated minimum and maximum recommended dos [8]. The orchard was treated in accordance with the guidelines of integrated production.
Thus, during the treatment with pesticides of apples were ud solutions 0.025% and 0.015% of myclobutanil, which reprent maximum and minimum recommended dos. The application of pesticides was done through a tractor in which two sprays were mounted. The samples were collected randomly in different interval days after application in accordance with European Commission Directive 2002/63/EC. All samples were placed in polythene bags, labelled and transported to the laboratory for further processing. Transportation and handling of apples was done through cooling boxes, the temperature of which did not exceed 5 to 6 degree Celsius.
2.2 Extraction and Clean-up
The extraction and purification of samples was bad on QuEChERS method developed by Anasstasiades et al. [9] 10 g homogenized sample was weighted into a 50 mL polypropylene centrifuge tube followed by addition of 10 mL acetonitril (MeCN) and 100 µL internal standard (carbofuran d-3). After the samples were mixed by vortexing 4g anhydrous sulfate (MgSO4), 1 g sodium chloride (NaCl), 1 g trisodium citrate dihydrate, 0.5 g disodium hydrogencitrate squihydrate was added and the tubes were shaken again 1 min and then were centrifuged at 3,000 g for5 min. Six milliliter of upper layer (acetonitril extract) was transfered into a 15 mL PP centrifuge tube containing PSA sorbent and anhydrous sulfate. After the last centrifugation at 3,000 g the supernatant was filter and transferred in vial for LC-MS/MS analysis.
2.3 Chemicals and LC-MS/MS Parameters
All solvents were of chromatography grade and were purchad from J. T. Baker (Deventer, Netherland). The standard pesticides were purchad from Dr. Ehrenstorfer (Augsburg, Germany), most of them had the purity ≥98%. Internal Standard (carbofuran d-3) was purchad from Pestanal, Fluka (Germany). Its purity was 99.7%.
The analys of pesticides were performed through the Agilent 1200 LC-MS/MS system (Agilent tec
hnology, USA) in positive mode Electrospray Ionization (+ESI). The mass analysis was carried out with an Agilent 6410 Triple Quadrupole mass spectrometer equipped with multi mode ion source. MassHunter Workstation B.06.00 (Agilent technology 2010) was ud for instrument control and data collaction. The chromatography paration was carried out on a Zorbax Ecllip XDB C18 column (50 × 4.6 mm, 1.8 μm) maintained at 30 °C.
The mobile pha consisted of methanol (30% v/v) and Milli-Q water (70% v/v) acidified with formic acid (solution 0.1%). Flow rate was t at 0.400 mL/min, the injection volume was 5 µL and the run time 26 min. The ESI source parameters were as follow: gas temperature (N2) 325 °C, gas flow rate 5 L/min, nebulizer pressure 40 psi and capillary voltage 2,000 v. The detection was performed using the multiple reactions monitoring mode (MRM).
2.4 Calibration Curve
Calibration curve was determined at five calibration level 0.005, 0.01, 0.025, 0.05 and 0.1 µg mL-1. Fig. 1 prents a good linearity with the correlation coefficient (R) above 0.99.
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Fate of Myclobutanil Residues after Application on Apples Growing to Korça District, Albania83
3. Results and Discussion
lagerfeldThe obtained data on pesticide residues of the conducted experiment with application of myclobutanil in apple tree to control fungal dia on fruit were compared to the MRLs t in EU regulations.
The MRM chromatogram showed for myclobutanil a retention time equal to 17.588 min. Confirmation and quantification of myclobutanil was done using m/z 289.2 ->70.2 dhe m/z 289.2 ->125.1 (Fig. 2).
Thus, the data prented in Table 1 and Fig. 3 showed that all the samples collacted immedialtely after the pesticide appliciaton had the highest level of myclobutanil residues and by the time a significant degradation of pesticide was obrved.
Thus, the level of myclobutanil residues varies from 0.928 mg kg-1 to 0.019 mg kg-1 and from 2.085 mg kg-1to 0.084 mg kg-1in Starking with the minimum and maximum applied dos at 1st and 40th day after application, respectively.
Also, the data on Table 2 indicate that in the Golden Delicious cultivar the level of myclobutanil resid
ues ranges from 0.878 mg kg-1 to 0.023 mg kg-1 and from 1.760 mg kg-1 to 0.055 mg kg-1 with the minimum and maximum applied dos at 1st and 40th day after application, respectively.
Therefore, the samples treated with maximum recommended do did not reach the MRL (0.6 mg kg-1) [10] before the 14th day after application, meanwhile the samples treated with minimum recommended do reached MRL before 7th day after application (e Fig.
3 and Fig. 4).
Fig. 1 Calibration curve of myclobutanil. All Rights Rerved.
Fate of Myclobutanil Residues after Application on Apples Growing to Korça District, Albania 84
Fig. 2 MRM chromatogram of myclobutanil standard solution (0.1 µg L-1).
Table 1 Residues levels of myclobutanil (mg kg-1) in Starking cultivar.
Days
Starking min. Starking max.
Year Mean Year
Mean 2015 2016 2015 2016
1 0.920 0.936 0.928 2.01美国第一任总统
2 2.159 2.085
6 0.539 0.545 0.542 0.730 1.563 1.146
14 0.197 0.339 0.268 0.419 0.747 0.583
21 0.075 0.090 0.083 0.350 0.495 0.422
28 0.034 0.023 0.028 0.104 0.218 0.161
40 0.028 0.011 0.019 0.066 0.105 0.086 All Rights Rerved.
Fate of Myclobutanil Residues after Application on Apples Growing to Korça District , Albania 85
Fig. 3 Degradation of myclobutanil in Starking cultivar.
Table 2 Residues levels of myclobutanil (mg kg -1) in Golden Delicious cultivar.
Days
Golden min.
Golden max. Year Mean Year Mean 2015 2016
福尔摩斯 演绎法2015 2016 1
0.842 0.913 0.878 1.734 1.785 1.760 6 0593 0.472 0.532 0.830 1.402 1.116 14 0.268 0.173 0.220 0.454 0.800 0.627 21 0.072 0.056 0.064 0.311 0.479 0.395 28 0.026 0.025 0.026 0.057 0.127 0.092 40
0.023
0.021
0.022
0.040
0.070
0.055he是什么意思
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