Development and Validation of QuEChERS Method for Estimation of Chlorantraniliprole Residue in Vegetables
Authors are with Pesticide Residue Analysis Laboratory, Dept. of Entomology, Punjab Agricultural Univ., Ludhiana-141004, Punjab, India. Direct inquires to author Mandal (E-mail: ). Journal of Food Science
(Impact Factor: 1.7).
07/2012; 77(12). DOI: 10.1111/j.1750-3841.2012.02801.x
An easy, simple and efficient analytical method was standardized and validated for the estimation of residues of chlorantraniliprole in different vegetables comprising brinjal, cabbage, capsicum, cauliflower, okra, and tomato. QuEChERS method was used for the extraction and cleanup of chlorantraniliprole residues on these vegetables. Final clear extracts of ethyl acetate were concentrated under vacuum and reconstituted into high performance liquid chromatograph (HPLC) grade acetonitrile, and residues were estimated using HPLC equipped with PDA detector system, C18 column and confirmed by liquid chromatograph mass spectrometer (LC-MS/MS), and high performance thin layer chromatograph (HPTLC). HPLC grade acetonitrile:water (80:20, v/v) was used as mobile phase @ 0.4 mL/min. Chlorantraniliprole presented distinct peak at retention time of 9.82 min. Consistent recoveries ranging from 85% to 96% for chlorantraniliprole were observed when samples were spiked at 0.10, 0.25, 0.50, and 1.00 mg/kg levels. The limit of quantification of this method was worked out to be 0.10 mg/kg.
Practical Application: The QuEChERS sample preparation is suitable for determination of chlorantraniliprole in brinjal, cabbage, capsicum, cauliflower, okra and tomato and thus demonstrating the great versatility of this method. The proposed analytical method using liquid chromatography techniques for the determination of chlorantraniliprole in different vegetable matrices has been demonstrated to be sensitive, fast, precise, accurate, and robust and can be used to monitor chlorantraniliprole residues in different vegetables.
Available from: Guy Smagghe
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Pollinators such as the bumblebee, Bombus terrestris, fulfil a crucial role in agriculture. In this context, tests were conducted with the insecticide chlorantraniliprole (Coragen®) as a model compound active on the ryanodine receptor of insects.
Chronic oral exposure via pollen induced lethargic behaviour in B. terrestris workers and their offspring (drones). Indeed, in nests exposed to 0.4 mg L(-1) , representing 1/100 of the concentration recommended for use in the field, workers and drones did not take their defensive position upon stimulation and they were less active than non-exposed insects. The different risk assessment tests used here demonstrated that contact and pollen exposure had no effect on bumblebee worker survival, whereas oral exposure via sugar water caused both acute (72 h LC50 = 13 mg L(-1) ) and chronic (7 week LC50 = 7 mg L(-1) ) toxicity. Severe sublethal effects on reproduction were recorded in nests orally exposed to pollen treated with chlorantraniliprole.
The present study identified an important physiological endpoint of sublethal effects on reproduction, as this is associated with lethargic behaviour after oral intake. As such, this is a factor that should now be incorporated into future risk assessments. Secondly, it confirmed that the assessment of sublethal effects on behaviour is needed for adequate risk assessment of 'potentially deleterious' compounds with a neurogenic target, as is also pointed out in the recent European Food Safety Authority (EFSA) guidelines.
Available from: Ramesh Arora
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ABSTRACT: The persistence pattern of chlorantraniliprole on berseem leaves and its risk assessment for the safety of cattle were studied. QuEChERS method was used for the extraction and cleanup of samples and the residues of chlorantraniliprole were estimated using high performance liquid chromatography (HPLC) and confirmed by Liquid Chromatograph–Mass Spectrometer (LCMS–MS). The dissipation studies on berseem were carried out by application of chlorantraniliprole at five different dosages i.e. 11.6, 17.1, 23.1, 34.7 and 46.2 g a.i. ha−1. Average initial deposits of chlorantraniliprole were found to be 0.47, 0.61, 0.78, 1.15 and 1.31 mg kg−1, respectively. The residues reached below determination limit (BDL) of 0.01 mg kg−1 in 5, 7, 7, 10 and 10 days for 11.6, 17.1, 23.1, 34.7 and 46.2 g a.i. ha−1 dosages, respectively. Half-life (t1/2) of chlorantraniliprole on berseem was observed to be 0.93, 1.14, 1.06, 1.00 and 1.33 days, respectively, at 11.6, 17.1, 23.1, 34.7 and 46.2 g a.i. ha−1. It was found that the theoretical maximum residue contributions (TMRC) values reached below maximum permissible intake (MPI) on 0 day in berseem samples treated with chlorantraniliprole. These studies, therefore suggest that the use of chlorantraniliprole formulation at different dosages does not seem to pose any hazards to the consumers and a waiting period of one day is suggested to reduce the risk before consumption of berseem leaves. These data could provide guidance for the proper and safe use of this pesticide on berseem in India.
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ABSTRACT: Off-target deposits of agrochemicals impose a general risk for the environment while environmental factors such as rainfall might cause significant pesticide removal from agricultural crops and contribute to a requirement for a higher rate and frequency of applications in intensive agricultural systems. In the present study, we analyzed the impact of five tank-mix adjuvants (three organosilicones - one superspreader, one penetrating agent and one spreader-sticker - as well as one paraffinic oil and one vegetable oil with non-ionic surfactants) on the amount of active ingredient (AI) deposited, deposit characteristics at the microscale, and rain-induced removal of chlorantraniliprole from the hydrophobic leaf surfaces of wheat and maize. In addition, the cuticular penetration of the AI was determined on astomatous cuticles from the adaxial side of apple leaves. The tank-mix adjuvants with lower surface tension (organosilicone superspreader and organosilicone-based penetrating agent) caused a lower contact angle of sessile droplets, larger surface coverage, and higher AI amount on wheat and maize leaves. Heavy rain (5 mm h-1) removed zero to 60% of the chlorantraniliprole from wheat leaves, and 20-60% from maize leaves, the losses being more pronounced in those treatments with higher initial AI amount. Moreover, in wheat we observed a pronounced effect of the rain amount (5 mm or 10 mm) on the AI removal. Environmental scanning electron micrographs indicated the rain-induced displacement of the AI and adjuvants and their partial re-allocation within the droplet footprint. Moreover, the micrographs showed no residues in adjacent areas outside the primary droplet footprint. Cuticular penetration of chlorantraniliprole, which was demonstrated here for the first time, ranged from 15 to 30%, but no statistical differences (p ≤ 0.05) were found between the experimental groups. In summary, the evaluated tank-mix adjuvants positively influenced the AI amount and deposit formation of chlorantraniliprole on hydrophobic leaves. In the case of rain, the add-on value of adjuvants on retention and AI amount might be partially lost, since the highest wash-off was associated with the highest deposition; nevertheless, the AI concentration on the leaves after rain remained significantly higher, or in worst-case similar to, the control group. In specific cases, the cuticular penetration might be improved, while no information on stomatal infiltration and bio-efficacy is provided. Finally, we point to the need for further optimization of adjuvant-AI systems to increase both penetration and rainfastness, and in this way constrain AI losses and unnecessary environmental contamination.
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