Desiodo Flubendiamide Research Articles

Method validation, residue behaviour and dietary risk assessment of insecticides (cyantraniliprole, acetamiprid, flubendiamide and its metabolite, des-iodo flubendiamide) in or on broccoli using LC-MS/MS.

Residue behaviour and dietary risk assessment of cyantraniliprole, flubendiamide and acetamiprid in broccoli were carried out using the QuEChERS (quick, easy, cheap, effective, rugged and safe) technique coupled with LC-MS/MS. The QuEChERS technique was validated on parameters such as linearity, accuracy, precision, robustness, matrix effects, limit of quantification (LOQ), specificity, retention time and ion ratio as per SANTE (Directorate General for Health and Food Safety) guidelines to attest to the specificity, accuracy and precision of the analytical method in estimating insecticide residues in and on broccoli heads and cropped soil. The LOQ of the method for all three insecticides was 0.01 mg/kg. The initial deposits of cyantraniliprole, flubendiamide and acetamiprid reduced to half of its concentration in 1.873-2.354, 1.975-2.484 and 1.371-1.620 days, respectively. No residues were detected in broccoli-cropped soil at harvest time (30 days after last spray). The proposed maximum residue limits (MRLs) of 1.5, 0.5-0.9 and 2.0-3mg/kg for cyantraniliprole, flubendiamide and acetamiprid were calculated using the Organisation for Economic Co-operation and Development MRL calculator. The acute and chronic dietary risk assessment of the tested insecticides identified no appreciable dietary risk to the Indian population from the consumption of broccoli heads. The findings of no dietary risk highlight the importance of informed pesticide usage in broccoli and the proposed MRL derived from this study offers crucial guidelines for the regulatory authorities, ensuring the safety of broccoli consumption.

Dissipation pattern of flubendiamide residues on capsicum fruit (Capsicum annuum L.) under field and controlled environmental conditions

ABSTRACTThis investigation was undertaken to compare the dissipation pattern of flubendiamide in capsicum fruits under poly-house and open field after giving spray applications at the recommended and double doses of 48 g a.i. ha−1 and 96 g a.i. ha−1. Extraction and purification of capsicum fruit samples were carried out by the QuEChERS method. Residues of flubendiamide and its metabolite, des-iodo flubendiamide, were analyzed by high-performance liquid chromatography–photodiode array, and confirmed by liquid chromatography–mass spectrometry/mass spectrometry. Limit of quantification of the method was 0.05 mg kg−1, and recovery of the insecticides was in the range of 89.6–104.3%, with relative standard deviation being 4.5–11.5%. The measurement uncertainty of the analytical method was in the range of 10.7–15.7%. Initial residue deposits of flubendiamide on capsicum fruits grown under poly-house conditions were (0.977 and 1.834 mg kg−1) higher than that grown in the field (0.665 and 1.545 mg kg−1). Flubendiamide residues persisted for 15 days in field-grown and for 25 days in poly-house-grown capsicum fruits. The residues were degraded with the half-lives of 4.3–4.7 and 5.6–6.6 days in field and poly-house respectively. Des-iodo flubendiamide was not detected in capsicum fruits or soil. The residues of flubendiamide degraded to below the maximum residue limit notified by Codex Alimentarius Commission (FAO/WHO) after 1 and 6 days in open field, and 3 and 10 days in poly-house. The results of the study indicated that flubendiamide applied to capsicum under controlled environmental conditions required longer pre-harvest interval to allow its residues to dissipate to the safe level.

Dissipation pattern and risk assessment of flubendiamide on chili at different agro-climatic conditions in India.

Dissipation pattern and risk assessment of flubendiamide and its metabolite (desiodo flubendiamide) on chili were studied at four different agro-climatic locations of India at the standard and double dose at 60 and 120ga.i. ha(-1) at 10days interval. Quantification of residues was done on a high-performance liquid chromatograph (HPLC) with a photo diode array detector. The limit of quantification (LOQ) of this method was found to be 0.01mgkg(-1) while limit of detection (LOD) being 0.003mgkg(-1). Residues of flubendiamide were found to be below the determination limit in 15days at both the dosages in all locations. Half-life of flubendiamide when applied at 60 and 120ga.i. ha(-1) ranged from 0.85 to 1.80 and from 0.95 to 2.79days, respectively. On the basis of data generated under the All India Network Project on Pesticide Residues, a preharvest interval (PHI) of 1day has been recommended and the flubendiamide 480 SC has been registered for use on chili in India by the Central Insecticide Board and Registration Committee, Ministry of Agriculture, Government of India. The maximum residue limit (MRL) of flubendiamide on chili has been fixed by the Food Safety Standard Authority of India, Ministry of Health and Family Welfare, Government of India, as 0.02μgg(-1) after its risk assessment.

Determination of flubendiamide residues and its safety evaluation for usage in cardamom by liquid chromatography

Cardamom is a major export oriented commodity in the world and it is susceptible to infestation by various pests which cause considerable economic loss. It is necessary to adopt new chemical insecticides with novel modes of action which control pest infestations. Flubendiamide fits into integrated pest management programmes in a variety of crops and is widely used in crops like tomato, cabbage and brinjal for controlling Lepidoptera pests and it is effective when used for cardamom. The major concern is ensuring residue free pods and safe harvest of cardamom for human consumption to prevent any health hazard. The present study investigates the behaviour of flubendiamide in cardamom in the humid subtropical conditions of India. A rapid, simple and selective method has been developed to determine residues of flubendiamide and desiodo flubendiamide in green cardamom, cured cardamom capsule, cured cardamom black seed and soil. The flubendiamide residues were extracted using the QuEChERS principle with acetonit...

Persistence and dissipation of flubendiamide and its risk assessment on gherkin (Cucumis anguria L.)

A supervised open field trial was conducted to evaluate the dissipation pattern and risk assessment of flubendiamide in gherkin fruits following foliar application of Fame 480 SC at 60 and 120ga.i. ha(-1). Samples of gherkin fruits were drawn at different time intervals and quantified by HPLC-DAD. The maximum initial deposits of flubendiamide on gherkin were found to be 0.79 and 1.52mgkg(-1), respectively, at recommended and double the recommended doses. The dissipation pattern of flubendiamide followed a first-order kinetics with half-lives of 1.87 to 2.16days at 60 and 120ga.i. ha(-1), respectively. The limit of quantification of flubendiamide and desiodo flubendiamide was observed to be 0.01mgkg(-1) for gherkin fruit and soil substrates. Theoretical maximum residue contribution (TMRC) for flubendiamide was calculated and found to be well below the maximum permissible intake (MPI) on gherkin fruits. Thus, the application of flubendiamide at the recommended dose on gherkin fruits presents no human health risks and safe to consumers.

Safety evaluation of flubendiamide and its metabolites on cabbage and persistence in soil in different agroclimatic zones of India

Supervised field trials following good agricultural practices were conducted at the research farms of four agricultural universities located at four different agroclimatic zones of India to evaluate the persistence and dissipation of flubendiamide and its metabolite, des-iodo flubendiamide, on cabbage. Two spray applications of flubendiamide 480 SC of standard and double dose at the rate of 24 and 48 g a.i. ha(-1) were given to the crop at a 15-day interval, and the residues of flubendiamide 2 h after spray were found in the range of 0.107-0.33 and 0.20-0.49 mg kg(-1) at respective doses. Residue of des-iodo flubendiamide was not detected in any cabbage sample during study period. No residues were found in the soil samples collected from all treated fields after 15 days of application. On the basis of data generated under All India Network Project on Pesticide Residues, a preharvest interval (PHI) of 10 days has been recommended, and the flubendiamide 480 SC has been registered for its use on cabbage by Central Insecticide Board and Registration Committee, Ministry of Agriculture, Government of India. The maximum residue limit (MRL) of flubendiamide on cabbage has been fixed by the Ministry of Health and Family Welfare, Government of India, under Food Safety Standard Authority of India as 0.05 μg/g after its risk assessment.

Modification of the existing MRL for flubendiamide in strawberries

In accordance with Article 6 of Regulation (EC) No 396/2005, Greece, hereafter referred to as the evaluating Member State (EMS), received an application from Bayer CropScience Aktiengesellschaft to modify the existing MRL for the active substance flubendiamide in strawberries. In order to accommodate for the intended use of flubendiamide, Greece proposed to raise the existing MRL from the limit of quantification of 0.01* mg/kg to 0.2 mg/kg. The EMS drafted an evaluation report in accordance with Article 8 of Regulation (EC) No 396/2005, which was submitted to the European Commission and forwarded to EFSA. According to EFSA the data are sufficient to derive a MRL proposal of 0.2 mg/kg for the proposed use on strawberries. Adequate analytical enforcement methods are available to control the residues of flubendiamide and its metabolite (des-iodo flubendiamide) in strawberries. Based on the risk assessment results, EFSA concludes that the proposed use of flubendiamide on strawberries will not result in a consumer exposure exceeding the toxicological reference values and therefore is unlikely to pose a consumer health risk.

Dissipation of flubendiamide residues in/on cabbage (Brassica oleracea L.)

Residues of fubendiamide and its metabolite desiodo flubendiamide were estimated in cabbage and soil using high-performance liquid chromatography with UV-vis detector. The initial deposits of flubendiamide residues on cabbage were found to be 0.16 and 0.31 μg g(-1) following two applications of flubendiamide 20 WG at 12.5 (standard dose) and 25 (double dose) g a.i. ha(-1) respectively at 10-days interval. The half-life values (t(1/2)) of flubendiamide on cabbage ranged from 3.4 to 3.6 days. When flubendiamide applied at both the standard and double dose, no detectable residues were found in cabbage and soil at harvest. Thus, a waiting period of 1.63 days was suggested for the safe consumption of flubendiamide-treated cabbage. These data could provide guidance for the proper and safe use of this pesticide on cabbage crops in India.

Simple and Rapid Method for Determination of Flubendiamide and its Residues in Soil and Water by HPLC-UV Detection

A simple and rapid method for the analysis of flubendiamide and its major metabolite desiodo flubendiamide, in soils and water with acetonitrile and ethyl acetate, respectively, is presented. Quantification was performed by reversed phase HPLC with UV detector. Mean recoveries of flubendiamide and desiodo flubendiamide in soils ranged from 88.01- 90.26 % and 90.5-92.29 % respectively. The applicability of the method to the determination of flubendiamide and desiodo flubendiamide in spiked water at three pH levels (4, 7 and 9.2) was evaluated. Recoveries for flubendiamide and desiodo flubendiamide spiked water were in the ranges 89.21-92.32 % and 92.2-95.57 % respectively. The detector linearity and the repeatability of the method were very precise.

Dissipation of Flubendiamide in/on Okra [Abelmoschus esculenta (L.) Moench] Fruits

A field experiment was undertaken at Indian Agricultural Research Institute, New Delhi during kharif (rainy season) in the year 2010 to evaluate the residue persistence of flubendiamide in/on okra fruits following foliar application of Belt 39.35% SC formulation at 24 (standard dose) and 48 (double dose) g a.i. ha(-1). After HPLC analysis study revealed that residues of flubendiamide in/on okra persisted till 5th and 7th day after the last spray at standard and double dose, respectively. The residues of flubendiamide were reported as parent compound, and des-iodo flubendiamide, a metabolite (photo product) of flubendiamide, was not detected in/on okra at any time during the study period. The initial deposits of 0.28 and 0.53 μg g(-1) in/on okra fruits reached below determination level of 0.01 μg g(-1) on the 7th and 10th day at standard and double dose, respectively. The half life of flubendiamide in/on okra fruits ranged from 4.7 to 5.1 days at standard and double dose, respectively. Soil sample collected from the treated field on the 15th day after the last spray revealed residues of flubendiamide or its metabolite below determination level (0.01 μg g(-1)) at single and double dose.

Persistence and Dissipation of the Insecticide Flubendiamide and its Metabolite Desiodo Flubendiamide Residues in Tomato Fruit and Soil

A method for residue analysis of flubendiamide and its metabolite desiodo flubendiamide was developed using high performance liquid chromatography. This method was then used to evaluate the residual level and dissipation rate of flubendiamide and desiodo flubendiamide in the tomato fruit. The half-life of flubendiamide in tomato fruit was 1.64 and 1.98 days in recommended and double of the recommended dose, respectively. Tomato fruit and soil samples analyzed on the 10th day after the last spray revealed that flubendiamide and its metabolite desiodo flubendiamide residues at below determination level (0.01 μg g(-1)) at either dose of application.

Flubendiamide Transport Through Packed Soil Columns

Flubendiamide insecticide is widely used in Indian subtropical condition to control lepidopteron pests mainly in rice and cotton. The present study reports leaching behaviour of flubendiamide, N(2)-[1,1-dimethyl-2-(methylsulfonyl)ethyl]-3-iodo-N(1)-[2-methyl-4-[1,2,2,2-tetrafluoro-1 (trifluoromethyl)ethyl] phenyl]-1,2-benzene dicarboxamide, in packed soil columns under different rainfall conditions. Flubendiamide did not leach out of the 25 cm long soil columns even after percolating water equivalent to 462.18 mm rainfall. After leaching with water equivalent to 462.18 mm rainfall, in analytical grade treatment, 68.06% of the recovered flubendiamide was the major amount present in 5-10 cm depth whereas in the formulation 67.22% of the recovered flubendiamide was confined to 0-5 cm depth. Results revealed that with percolating 160 mL of water residues of desiodo flubendiamide detected up to 20-25 cm layer along with 9.47% residues in this layer, indicating that metabolite is more mobile as compared to analytical grade flubendiamide and 39.35% SC formulation. Formulation slowed the downward mobility of flubendiamide in soil column. Flubendiamide is slightly mobile in sandy loam soil, but desiodo flubendiamide is relatively more mobile and may leach into ground water.

Dissipation pattern of flubendiamide in/on brinjal (Solanum melongena L.)

Residues of flubendiamide and desiodo flubendiamide were studied following three applications of flubendiamide 480 SC at 7 days interval at 90 and 180 g a.i. ha(-1) in/on brinjal fruits. An average initial deposit of 0.33 and 0.61 mg kg(-1) of flubendiamide was observed respectively after application at single and double dosages. The residues of flubendiamide dissipated quickly at both the dosages, and after 3 days, the extent of dissipation was found to be about 76% and 79% at the single and double dosages, respectively. Brinjal fruit samples analysed at different time intervals did not show the presence of desiodo flubendiamide. The half-life of flubendiamide was observed to be 0.62 and 0.54 days at single and double dosages, respectively. The limit of determination of flubendiamide and desiodo flubendiamide was observed to be 0.05 mg kg(-1). Soil samples analysed after 15 days of the last application did not reveal the presence of flubendiamide and desiodo flubendiamide at their determination limit of 0.05 mg kg(-1). An assessment of the total intake of flubendiamide resulting through the consumption of brinjal fruits and its comparison with acceptable daily intake seems to be quite safe from consumer point of view.

Simultaneous Determination of Flubendiamide its Metabolite Desiodo Flubendiamide Residues in Cabbage, Tomato and Pigeon Pea by HPLC

A sensitive and simple method for simultaneous analysis of flubendiamide and its metabolite desiodo flubendiamide in cabbage, tomato and pigeon pea has been developed. The residues were extracted with QuEChERS method followed by dispersive solid-phase extraction with primary secondary amine sorbent to remove co extractives, prior to analysis by HPLC coupled with UV-Vis detector. The recoveries of flubendiamide and desiodo flubendiamide were ranged from 85.1 to 98.5% and 85.9 to 97.1% respectively with relative standard deviations (RSD) less than 5% and sensitivity of 0.01 μg g(-1). The method offers a less expensive and safer alternative to the existing residue analysis methods for vegetables.

Residual behaviour and risk assessment of flubendiamide on Chickpea ( Cicer arietinum L.)

The study was undertaken to determine the disappearance trends of flubendiamide residues on chickpea under field conditions and thereby, ensure consumer safety. Average initial deposits of flubendiamide on chickpea pods were found to be 0.68 and 1.17 mg kg −1, respectively, following three applications of flubendiamide 480SC @ 48 and 96 g a.i. ha −1 at 7 d intervals. Half-life of flubendiamide on chickpea pods was observed to be 1.39 and 1.44 d, respectively, at single and double dosages whereas with respect to chickpea leaves, these values were found to be 0.77 and 0.86 d. Desiodo flubendiamide was not detected at 0.05 mg kg −1 level on chickpea samples collected at different intervals. Theoretical maximum residue contribution (TMRC) for flubendiamide was calculated and found to be well below the maximum permissible intake (MPI) on chickpea pods and leaves at 0-day (1 h after spraying) for the both dosages. Thus, the application of flubendiamide at the recommended dose on chickpea presents no human health risks and is safe to the consumers.

Comparative persistence of flubendiamide residues in chilli following application as individual and combination formulation

Introduction Chilli, an important crop of India, is infested by various insect pests during its cultivation. A new insecticide flubendiamide is being registered in India individually as well as in combinationwith thiacloprid for use against lepidopteran and sucking pests of chilli. Objectives To study the dissipation pattern of flubendiamide following its application as flubendiamide alone and in combination with thiacloprid. Methods Standardized methodologies using high-performance liquid chromatography, were adopted to estimate residues of flubendiamide, its metabolite, des-iodo flubendiamide and thiacloprid in chilli. Results Average initial deposits of flubendiamide in chilli following its application as flubendiamide alone or as flubendiamide and thiacloprid combination were almost the same, i.e. 0.467 and 0.499mgkg � 1 , respectively, from treatment at recommended dose of 60ga.i.ha � 1 , 0.824 and 0.992mgkg � 1 from treatment at double the recommended dose. Residues dissipated to below detectable levels within 7‐10 days, respectively. Des-iodo flubendiamide, a metabolite of flubendiamide was not detected in any of the chilli samples collected at different time intervals. Residues of thiacloprid also dissipated quickly and were below quantifiable level of 0.01mgkg � 1 at 7 and 10 days, respectively. Conclusion Flubendiamide residues behaved in almost identical manner when applied alone or in combination with thiacloprid. SHARMA D, MOHAPATRA S, AHUJA AK, DIVAKAR JV, DEEPA M (2011). Comparative persistence of flubendiamide residues in chilli following application as individual and combination formulation. Quality Assurance and Safety of Crops & Foods, 3, 69‐73.

Development of an analytical method for analysis of flubendiamide, des-iodo flubendiamide and study of their residue persistence in tomato and soil

Flubendiamide is a new insecticide that has been found to give excellent control of lepidopterous pests of tomato. This study has been undertaken to develop an improved method for analysis of flubendiamide and its metabolite des-iodo flubendiamide and determine residue retention in tomato and soil. The analytical method developed involved extraction of flubendiamide and its metabolite des-iodo flubendiamide with acetonitrile, liquid-liquid partitioning into hexane-ethyl acetate mixture (6:4, v v−1) and cleanup with activated neutral alumina. Finally the residues were dissolved in gradient high pressure liquid chromatography (HPLC) grade acetonitrile for analysis by HPLC. The mobile phase, acetonitrile-water at 60:40 (v v−1) proportion and the wavelength of 235 nm gave maximum peak resolution. Using the above method and HPLC parameters described, nearly 100 % recovery of both insecticides were obtained. There was no matrix interference and the limit of quantification (LOQ) of the method was 0.01 mg kg−1. Initial residue deposits of flubendiamide on field-treated tomato from treatments @ 48 and 96 g active ingredient hectare−1 were 0.83 and 1.68 mg kg−1,respectively. The residues of flubendiamide dissipated at the half-life of 3.9 and 4.4 days from treatments @ 48 and 96 g a.i. ha−1, respectively and persisted for 15 days from both the treatments. Des-iodo flubendiamide was not detected in tomato fruits at any time during the study period. Residues of flubendiamide and des-iodo flubendiamide in soil from treatment @ 48 and 96 g a.i. ha−1 were below detectable level (BDL, < 0.01 mg kg−1) after 20 days. Flubendiamide completely dissipated from tomato within 20 days when the 480 SC formulation was applied at doses recommended for protection against lepidopterous pests.

Persistence and Dissipation of Flubendiamide and Des-iodo Flubendiamide in Cabbage (Brassica oleracea Linne) and Soil

Flubendiamide belongs to a novel class of insecticide which controls lepidopteran pest complex of cabbage such as diamondback moth, cabbage white butterfly, cluster caterpillar etc. Being a newly introduced insecticide no information is available on its residue persistence in cabbage. A study was undertaken to evaluate the residue persistence of flubendiamide in cabbage and soil following 2 applications of flubendiamide 480 SC at the recommended and double the recommended dose of 24 and 48 g a.i. ha(-1). Initial residue deposits of flubendiamide in cabbage were 0.33 and 0.49 mg kg(-1) respectively. The residues persisted for 10 days from the both the treatments and dissipated with the half-life of 3.9 and 4.45 days, respectively. Des-iodo flubendiamide, a metabolite of flubendiamide, was not detected in cabbage at any time during the study period. Soil sample collected from the treated field after 15 days was free from any residue of flubendiamide or its metabolite.

Dissipation kinetics of flubendiamide and thiacloprid on tomato (Lycopersicon esculentum Mill) and soil

Introduction Flubendiamide, a phthalic acid diamide widely used against the lepidopteran pests and thiacloprid, the first chloronicotinyl insecticide quite effective against the sucking insects, white flies and jassids have recently been used on various vegetable crops in India. Objectives Studies on dissipation kinetics of insecticides is very essential to work out their half- lives and waiting periods for the safe consumption of agricultural produce. Methods Standardized methodology supported by recovery studies is adopted to estimate residues of flubendiamide and thiacloprid on tomato. Final estimation of residues was accomplished using high performance liquid chromatography by employing C18 column and photo diode array at 230 wavelength. Results Half-lives values for flubendiamide following its three applications at 10 days intervals @ 48 g a.i. ha−1 were observed to be 0.33 and 1.00 days, respectively. Similarly, at the same application rate these values for thiacloprid were found to be 1.18 and 0.95 days, respectively. Flubendiamide and thiacloprid residues were observed to dissipate below their determination limit of 0.01 mg kg−1 after 3 and 5 days, respectively, when applied @ 48 g a.i.ha−1. Soil samples collected after 15 days did not show the presence of flubendiamide, desiodo flubendiamide, and thiacloprid at their determination limit of 0.01 mg kg−1. Conclusion A waiting period of 5 days is recommended for safe consumption of tomato fruit after application of combination formulation of flubendiamide 24%+thiacloprid 24% (480 SC) @ 200 g ha−1.

Dissipation Kinetics of Flubendiamide on Chili and Soil

Average initial deposits of flubendiamide on chili were found to be 1.06 and 2.00 mg kg(-1), respectively, following two applications of flubendiamide 480SC at 60 and 120 g a.i. ha(-1) at 10 days interval. More than 80% of flubendiamide residues dissipated just after 3 days of the last application at both the dosages. Residues of flubendiamide dissipated below detectable level of 0.01 mg kg(-1) in 7 and 10 days at single and double dosages, respectively. Half-life (t(1/2)) of flubendiamide on chili was observed to be 0.96 and 0.91 days, respectively, at single and double dosages. Desiodo flubendiamide was not detected at 0.01 mg kg(-1) level in chili samples collected at different time intervals. Red chili and soil samples collected after 20 days did not reveal the presence of flubendiamide or its metabolite desiodo flubendiamide.