Development and validation of a confirmative LC-MS/MS method for the determination of ß-exotoxin thuringiensin in plant protection products and selected greenhouse crops

2012 ◽  
Vol 405 (5) ◽  
pp. 1631-1639 ◽  
Author(s):  
Theo C. de Rijk ◽  
Ruud C. J. van Dam ◽  
Paul Zomer ◽  
Ed A. M. Boers ◽  
Pieter de Waard ◽  
...  
2021 ◽  
Author(s):  
Mathavan Vickneswaran ◽  
James Carolan ◽  
Blanaid White

The expanding nature of the agricultural sector has fuelled the intensification of plant protection products usage, including pesticides. These pesticides may persist in soils, necessitating their accurate determination in a...


2020 ◽  
Vol 64 (3) ◽  
pp. 150-157
Author(s):  
Valeriy N. Rakitskii ◽  
Ngoc Hai Doan ◽  
Nataliya E. Fedorova ◽  
Irina V. Bereznyak ◽  
Van Tung Lo ◽  
...  

Introduction. From the evaluation of the positions of residual quantities of pesticides, the hygienic safety assessment of imported food products is most relevant under the current agreement on a free trade zone between the EAEU and the Socialist Republic of Vietnam, as well as in connection with a large list of chemical plant protection products used during the vegetation of crops. The purpose of the study. Rating the level of residual quantities of pesticides in samples of selected food products produced in Vietnam is the purpose of the study. Research objectives. To quantify 42 active ingredients of pesticides (and their metabolites) in samples of rice grain, dragon fruit (pitahaya), avocado, mango and banana (fresh and dried) are the research objectives. Material and methods. Multicomponent and individual methods based on LC and GC with MS-detection and FLD were used to identify active ingredients of pesticides. The sample preparation procedure with QuEChERS technology was used for the multi residues determination of the 40 compounds. The determination of avermectins (abamectin and emamectin benzoate) was carried out after the conversion of substances into fluorogenic derivatives. Results. Residual amounts of tebuconazole (rice - 0.53 ppm, mangoes - 0.26 ppm, avocado - 0.15 ppm), fludioxonil (rice - 0.017 ppm), imidacloprid (dried mangoes - 0.01 ppm), carbendazim (dried mangoes - 0.011 ppm) were identified in single samples No residual avermectins have been identified. The content of substances in the analyzed samples of dragon fruit (pitahaya) did not exceed 0.01 ppm. Discussion. The results obtained in the work are compared with the data of the annual pan-European and national monitoring, information on which is publicly available (2017), including imported goods, according to which rice and dragon fruits as objects of monitoring are given increased attention. Conclusions. The safety of certain types of food products imported from Vietnam is shown by the content of residual quantities of pesticides.


Molecules ◽  
2019 ◽  
Vol 24 (12) ◽  
pp. 2203 ◽  
Author(s):  
Ewa Szpyrka ◽  
Maciej Thomas ◽  
Magdalena Podbielska

The aim of this study was the modification and application of the QuEChERS method for the preparation and purification of samples in order to determine the level of captan in real wastewater originating from a plant protection products factory which was characterized by a significant content of organic substances [Chemical Oxygen Demand (COD) = 856 ± 128 mg O2/L and Total Organic Carbon (TOC) = 62 ± 9 mg/L]. The optimization of the method consisted of the selection of solvents used for the extraction of captan from wastewater and also sorbents used to purify the extracts by the dispersion of a solid phase extraction technique (dSPE). Two steps were used: extraction and clean-up. In the extraction step, acetonitrile was replaced by anacetonitrile:acetone mixture. In the clean-up step by the dSPE, five sorbents were tested: Florisil®, aluminum oxide (Al2O3), zirconium oxide (ZrO2), silicon oxide (SiO2) and PSA (primary and secondary amine). Concentrations of captan in wastewater extracts were determined by gas chromatography (GC) combined with electron capture detection (μECD). The best recovery parameters and precision of the method were obtained for samples purified using ZrO2 (recovery 98% and precision expressed as relative standard deviation RSD 8%) and Florisil® (recovery 96%, RSD 9%). Limits of detection (LOD) and quantification (LOQ) for determination of captan in diluted extract of wastewater were 0.003 and 0.01 mg/L, respectively. Matrix effects were in the range of −69% to −44% for samples purified by ZrO2 and Florisil®, respectively. The modified and optimized method was applied for fast and simple determination of captan levels in real industrial wastewater samples, in which the concentration of captan in diluted extract was determined to be 4.0 ± 0.3 mg/L.


2021 ◽  
Vol 17 (2) ◽  
pp. 96-101
Author(s):  
О.М. Korshun ◽  
А.О. Lipavska ◽  
D.S. Milokhov ◽  
А.О. Аvramchuk ◽  
S.T. Omelchuk

Relevance. To date, there are no approved methods in Ukraine for the determination of azoxystrobin, thiabendazole, fludioxonil and pyridate in grain chickpeas. Therefore, there is a need for scientific substantiation of the method selection, the development of conditions for sample preparation of chickpea grain, qualitative identification and quantification of pesticides in this matrix used in protection system of chickpea was given in the article, which will allow to control the established hygienic standards of pesticides and minimize pesticide negative impact on population health and the environment. Objective of the research is to develop methods for the determination of azoxystrobin, thiabendazole, fludioxonil and pyridate in grain chickpea. Materials and methods. Chromatographic analysis was performed by Shimazu (Japan) liquid chromatographs using ultraviolet and fluorescent detection. The package of IBM SPSS StatisticsBase v.22 and MS Exel statistical programs was used for statistical processing of results. Results. Optimal conditions of sample preparation of chickpea grain and chromatographic determination of azoxystrobin, fludioxonil, thiabendazole and pyridate (as the sum of pyridate and its metabolite – pyridafol) with the limits of quantitative determination of 0.1; 0.1; 0.01 and 0.05 mg/kg, respectively, wеre developed to provide the determination of the analyzed compounds at the required level (the measure of correctness is (72–75)%) and the control of the established hygienic standards of these compounds in chickpea grain. Conclusions. Developed methods for determination of azoxystrobin, fludioxonil, thiabendazole and pyridate in chickpea grain by high-performance liquid chromatography allow to control the established hygienic standards, to obtain representative information on the content of pesticide residues, which is a prerequisite for risk assessment of plant protection products.


Author(s):  
Asbjørn Magne Nilsen ◽  
Hubert Dirven ◽  
Jan Ludvig Lyche ◽  
Marit Låg ◽  
Katrine Borgå ◽  
...  

MCPA (4-chloro-2-methylphenoxyacetic acid) is the active ingredient in several registered herbicides. VKM concluded in 2006 that the effects observed in experiments with dogs were of little relevance to humans, and an AOEL value of 0.036 mg/kg bw/day was proposed, based on renal effects in a 90-day study in rats. The manufacturer is of the opinion that AOEL should be set to 0.11 mg/kg bw/day, and ADI to 0.05 mg/kg bw/day, based on the view that since a 90-day and 2-year study in rats were conducted in the same lab using the same rat strain, it is reasonable to eliminate effects which are not reproduced in both sets of data. The Norwegian Food Safety Authority has therefore requested VKM’s Panel for Plant Protection Products for an opinion on the determination of NOAEL values based on the 90-day and 2-year studies in rats, and consider if it is acceptable to use the manufacturer's approach for an overall consideration of the submitted studies. The Panel has discussed the findings in the two rat studies and concluded that it is not considered acceptable that individual studies separated by several years, in this case studies performed in 1985 and 1988, are taken together and data not reproduced in both sets eliminated. The Panel is still of the opinion that both AOEL and ADI for MCPA should be set to 0.036 mg/kg bw/day based on a NOAEL of 3.6 mg/kg bw/day (50 ppm) from assessment of the renal effects in the 90-day study in rats. The manufacturer has also requested a reconsideration of the present values for dermal absorption which was set by the Norwegian Food Safety Authority during the administrative review of the product MCPA 750 Liquid in 2013. VKM’s Panel on Plant Protection Products supports the conclusion of the Norwegian Food Safety Authority concerning the determination of values for dermal absorption of MCPA. This includes the consideration of remaining substance in skin after washing as part of the absorbed dose in the in vitro studies, and the use of the same experimental time period in the in vitro and in vivo experiments as a basis for the so-called “Triple-pack-approach” for determination of human dermal absorption.


2019 ◽  
Vol 6 (2) ◽  
pp. 76-83
Author(s):  
V. Yaroshevsky

Aim. The main aim of the research was to compare different methods of fermentation medium energy effi ciency agitation. Methods. The analysis of mass transfer processes in fermenters using different methods of agitation was made. Experimental determination of energy consumption for medium agitation while using a mechanical agitator and an external circulation loop was realized. Estimation of energy effi ciency indices. Results. It was determined that energy effi ciency of agitation by circulation during the cycle of bacterial preparation Planriz BT (Biotechnica) exceeded mechanical agitation 1.3 times in case of aeration, and 2.6 times in the non-aeration mode. Conclusions. The method of agitation by circulation of fermentation medium using an external loop is more energy-effi cient compared to mechanical agitation even in the case of using a slow-speed agitator.


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