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In the present work we have studied photo-induced decomposition of iprodione on silica support with different additions of titanium dioxide. Both the experimental and theoretical (DFT) approaches have been applied. It was found that 16 hours visible light exposure of the samples with 0.1% and 1.0% of TiO 2 leads respectively to 48.28% and 21.05% of residual amounts of iprodione in these samples. A number of intermediates and end products were identified by means of GS-MS and LC-MS chromatography. The iprodione isomer (RP 30228) and its decay product 1-(3,5-dichlorophenyl)-5-isopropyl biuret (RP 36221) were identified among them. Our DFT calculations have revealed the detailed mechanisms of formation of the above products and the mechanism of accelerated proton-induced decomposition of iprodione molecules adsorbed on the TiO 2 surface. Also, the intra-molecular reasons for iprodione stability in acidic media were clarified together with the mechanism of hydantoin cycle opening under the action of hydroxyl anions.

In this study, we propose an improved analytical method for the multiresidue analysis of captan (plus its metabolite, tetrahydrophthalimide), folpet (plus its metabolite, phthalimide), captafol, and iprodione in cereals using liquid chromatography tandem mass spectrometry (LC-MS/MS). As captan, captafol, and folpet are easily degraded during homogenisation and extraction, samples were comminuted with liquid nitrogen, and both QuEChERS and ethyl acetate-based extraction workflows provided a satisfactory method performance. The optimised LC-MS/MS procedure with electrospray ionisation did not degrade these compounds, and offered sufficient method selectivity by resolving and minimising co-eluting matrix-derived interferences. The method also resolved the problem of non-specific mass spectra that these compounds usually produce on GC-MS analysis involving electron ionisation. The method performance was satisfactory for all 6 compounds at 0.01 mg kg -1 and higher levels of fortification, and validated as per the SANTE/11813/2017 guidelines of analytical quality control in a wide range of cereals including rice, wheat, sorghum, and corn. The method provides special advantage of simultaneous analysis of captan, and folpet along with their metabolites (tetrahydrophthalimide, and phthalimide, respectively) in combination with captafol, and iprodione in a single chromatographic run. Although iprodione is known to degrade to 3,5-dichloroaniline, since this metabolite is not a part of the residue definition, it was not included in the scope of this method. As the method demonstrates satisfactory selectivity, sensitivity, accuracy, precision, and robustness in a wide range of cereal matrices, it is recommended for regulatory testing of these compounds in cereals.

Iprodione is a fungicide widely used in viticulture in most agricultural countries. It was banned recently in the European community because of its carcinogenic and endocrine disrupting characters. In this work, a cheap analytical method able to monitor iprodione in a white wine was developed. Molecularly imprinted sol-gel polymers (MIS) specific to iprodione and using green solvents were synthesized. An experimental design having the following factors (solvent volume and crosslinker quantity) was used to prepare an optimal MIS. In terms of selectivity, the optimal MIS showed the best partition coefficient towards iprodione in a white wine containing four other competing fungicides (procymidone, pyrimethanil, azoxystrobin and iprovalicarb). A solid phase extraction method using the optimal MIS was optimized and applied to analyse iprodione in a white wine. Low detection and quantification limits were reached 11.7 and 39.1 µg/L respectively., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

This study reports the optimization of a binary dispersive liquid-liquid microextraction method for the determination of iprodione, procymidone, and chlorflurenol by gas chromatography mass spectrometry. The study was aimed at using two extraction solvents to increase the extraction efficiency of all analytes. The binary solvents recorded results higher than the mono-solvents. After examining the effects of main experimental parameters and their interactions by analysis of variance, 200 μL of binary mixture (dichloromethane and 1,2-dichloroethane), 2.5 mL of ethanol, and 15 s vortex were obtained as optimum parameters. The detection and quantification limits calculated for the analytes were found to be between 0.30-1.6 and 1.0-5.3 ng/mL, respectively. Enhancement in detection power calculated as a ratio of the binary extraction detection limit to the detection limit of direct GC-MS analysis was 105-, 214-, and 233-fold for chlorflurenol, iprodione, and procymidone, respectively. In order to check the accuracy of the developed method, recovery study was performed. Water sampled from a lake and two wastewater samples from treatment facilities were spiked at two concentrations, and the percent recovery calculated for the samples ranged between 87 and 116%. These results confirmed the suitability of the method to real samples for accurate determination of the analytes at trace levels.

A biopurification system based on the adsorption and degradation capacity of a biomixture to degrade a mixture of pesticides (atrazine, chlorpyrifos, iprodione; 50 mg kg -1 each) in repeated applications (0, 30, and 60 days) was evaluated. Tanks of 1 m 3 packed with a biomixture (ρ 0.29 g mL -1 ) with and without vegetal cover were used. The biomixture contained soil, peat, and wheat straw in a proportion 1:1:2 by volume, respectively. Pesticide concentrations, biological activities (urease, phenoloxidase, and dehydrogenase), and microbial community changes (DGGE and qPCR) were evaluated periodically. Pesticide dissipation was higher in tanks with vegetal cover (> 95%) and no variation was observed after the three applications; contrarily, pesticide dissipation decreased in the tank without vegetal cover after each application. The presence of vegetal cover decreased the half-life of pesticides by at least twice. Biological activities were in general not affected by the application and reapplication of pesticides in the same treatment; however, they exhibited some differences between tanks containing and lacking the vegetal cover. High similarity between microbial groups (actinobacteria, bacteria, and fungi) was observed, suggesting no influence ascribable to the successive pesticide applications. The number of copies of bacteria and actinobacteria remained almost constant during the assay. However, the number of copies of fungi was significantly higher in the uncontaminated tank without vegetal cover.

Field experiments were conducted in two different locations to determine the residue levels and dissipation rates of iprodione in tobacco leaves and soil. Iprodione 50% wettable powder formulation was sprayed once at 12.50 g/ha to study the dissipation behavior and three to four times at 8.33 g/ha (recommended dose) and 12.50 g/ha (1.5 times the recommended field dose) to determine the residue levels of iprodione in tobacco leaves and soil after repeated applications. Iprodione residues in both green tobacco leaves and soil dissipated to about 50% of the initial deposits after 7 days and then further dissipated to more than 90% after 35 days.The dissipation of iprodione followed first order kinetics and the calculated half-life values (T (1/2)) were 5.64-8.80 days in green tobacco leaves and 7.50-9.93 days in soil, respectively. Iprodione residue levels in flue-cured tobacco leaves 21 days after the third and fourth applications ranged from 7.61 to 40.98 mg/kg. Meanwhile, the residues detected in soil decreased to 0.010-0.117 mg/kg 21 days after the last treatment.

Background: Greenhouse tomato production is intended exclusively for fresh consumption. Typical greenhouse conditions provide a conducive environment for the development of different fungi, principally late blight and grey mould, that can destroy plants and fruits. For this reason, different fungicides with different sites of action are used in integrated pest management strategies. Famoxadone, fenamidone, fenhexamid and iprodione (fig. 1) are fungicides of difference classes with different actions that could be used to control tomato pests., Results: The QuEChERS method showed good recoveries, and the analytical method allowed good separation of the fungicides selected. Good results were obtained in terms of repeatability and intermediate precision, with a coefficient of variation of < 9.8%. The limits of determination and quantification of the method were far below the maximum residual levels (MRLs) set by the EU for these fungicides in tomatoes. The analysis of fungicide residues showed that cv. Shiren accounted for higher residue levels than cv. Caramba. The dissipation curves were similar in the two cultivars, indicating that the decrease in pesticides was not related to the tomato type., Conclusions: 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., (Copyright © 2011 Society of Chemical Industry.)

Iprodione is an agricultural fungicide that is difficult to detect in foods by HPLC because it coelutes with natural compounds in the food. We previously showed that food matrix could be degraded with titanium dioxide powder (TP). Here we describe an improved method for detection of iprodione using silica gel supported titanium dioxide (SGT). To synthesize SGT, titania-sol was mixed with diethanolamine, 2-propanol, and titanium tetraisopropoxide. After titania-sol was infiltrated into the silica gel (particle diameter 4 mm), the mixture was dried and then heated. Crude basil extract containing iprodione was mixed with SGT in a quartz vial, and the vial was irradiated with a UV light to selectively decompose the matrix interfering with the iprodione determination. In HPLC chromatograms of the treated solution, the interference peak decreased 35 times faster with SGT than with TP. When SGT (11 g) was added to the extract (20 mL) of dry basil (2 g), black light irradiation for 30 min was enough to quantify iprodione. The recovery rate of iprodione was 99.1%. Thus, the photocatalytic cleanup method using SGT is effective for analyzing residual iprodione in dry basil.

Titanium dioxide was used as a photocatalyst to decompose interfering substances for a quantitative analysis of a fungicide (iprodione) in dry basil by HPLC. A quartz vial containing basil extract and titanium dioxide was irradiated with black light. The interfering substances were almost completely decomposed by 180 min of irradiation, whereas 88.3% of iprodione remained. The recovery of iprodione was 102.6% by the proposed method in basil extracts. This may have been due to different decomposition rates of the analyte and interfering substances.

Two methodologies based on vibrational spectrometry--making use of Fourier transform infrared absorption (FTIR) and Raman spectrometry--were developed for iprodione determination in solid pesticide formulations. The FTIR procedure involved the extraction of iprodione by CHCl(3), and the latter determination involved measuring the peak area between 1450 and 1440 cm(-1), corrected using a horizontal baseline defined at 1481 cm(-1). FT-Raman determination was performed directly on the powdered solid products, using standard chromatography glass vials as sample cells and measuring the Raman intensity between 1003 and 993 cm(-1), with a two-point baseline correction established between 1012 and 981 cm(-1). The sensitivities obtained were 0.319 area values g mg(-1) for FTIR determination and 5.58 area values g g(-1) for FT-Raman. The repeatabilities, taken to be the relative standard deviation of five independent measurements at 1.51 mg g(-1) and 10.98% w/w concentration levels, were equal to 0.16% and 0.9% for FTIR and FT-Raman, respectively, and the limits of detection were 0.3 and 0.2% w/w (higher than those obtained for HPLC, 0.016% w/w). FTIR determination provided a sample frequency of 60 h(-1), higher than those obtained for the Raman and reference chromatography methods (25 and 8.6 h(-1), respectively). On the other hand, the new FT-Raman method eliminates reagent consumption and waste generation, and reduces the need for sample handling and the contact of operator with the pesticide. In spite of their lack of sensitivity, vibrational procedures can therefore provide viable environmentally friendly alternatives to laborious, time- and solvent-consuming reference chromatography methods for quality control in commercially available pesticide formulations.

This work reports on the fundamental characteristics of a commercial enzyme-linked immunosorbent assay (ELISA) for iprodione and the application to residue analysis in agricultural samples. The ELISA had enough analytical sensitivity (I50 value 4.0 ng g(-1); limit of detection 0.3 ng g(-1)) to determine a trace of iprodione residue and had a high selectivity. Only administering simple dilution of sample extracts very easily surmounted the most troublesome matrix interference in ELISA for pesticide residue analysis. Consequently, a rapid and simple detection method for iprodione was reached by the combination of the sample dilution and the devised extraction method in which it required no instruments for extraction. The average recovery values from spiked samples with the ELISA were between 106.4 and 115.8% with the average coefficients of variation between 3.0 and 4.0%. The results obtained with the ELISA correlated well with those by the reference chromatographic method for all tested agricultural samples (r>0.993). These findings strongly indicate that the proposed ELISA was an adequate and reliable detection method for iprodione residues.