In the present day scenario of increasing awareness and concern about the pesticides, it is very important to ensure the quality of data being generated in pesticide residue analysis. To impart confidence in the products, terms like quality assurance and quality control are used as an integral part of quality management. In order to ensure better quality of results in pesticide residue analysis, validation of analytical methods to be used is extremely important. Keeping in view the importance of validation of method, the validation of QuEChERS (quick, easy, cheap, effective, rugged, and safe) a multiresidue method for extraction of 13 organochlorines and seven synthetic pyrethroids in fruits and vegetables followed by GC ECD for quantification was done so as to use this method for analysis of samples received in the laboratory. The method has been validated as per the Guidelines issued by SANCO (French words Sante for Health and Consommateurs for Consumers) in accordance with their document SANCO/XXXX/2013. Various parameters analyzed, viz., linearity, specificity, repeatability, reproducibility, and ruggedness were found to have acceptable values with a per cent RSD of less than 10%. Limit of quantification (LOQ) for the organochlorines was established to be 0.01 and 0.05 mg kg for the synthetic pyrethroids. The uncertainty of the measurement (MU) for all these compounds ranged between 1 and 10%. The matrix-match calibration was used to compensate the matrix effect on the quantification of the compounds. The overall recovery of the method ranged between 80 and 120%. These results demonstrate the applicability and acceptability of this method in routine estimation of pesticide residues of these 20 pesticides in the fruits and vegetables by the laboratory.
The persistence of chlorpyrifos, fluopyram, and tebuconazole was estimated in green pods, matured seeds, and soil of French beans using dispersive QuEChERS. Three foliar applications each of chlorpyrifos and a combination fungicide fluopyram + tebuconazole (Luna experience, 400 SC) were applied at 600 and 125 + 125 as a standard dose and 1200 and 250 + 250 g a.i. ha as a double dose, respectively, were applied at an interval of 10 days and treated pods were picked up at regular intervals. Dried mature seeds and soil were also monitored at harvest. The initial deposits of chlorpyrifos on bean pods were 3.083 and 6.017 mg kg with a half-life of 1.86 and 2.29 days, at respective doses. Foliar application of a combi product Luna experience yielded 3.396 and 5.772 mg kg residues of fluopyram and 3.613 and 5.887 mg kg of tebuconazole in green pods at standard and double dose with almost same half-lives of 3.4 and 3.8-3.9 days. Residues declined below the limit of quantitation (LOQ) of 0.05 mg kg in green beans after 15 and 25 days after the application of double dose of chlorpyrifos and Luna experience, respectively. However, the residues in dry bean seeds and soil reached below the LOQ of 0.05 mg kg at the time of harvest. A pre-harvest interval of 5, 10, and 7 days has been proposed for chlorpyrifos, fluopyram, and tebuconazole, respectively, in beans. HQ < 1 and TMDI < MPI in all test chemicals. Hence, it was concluded that a waiting period of 5 days for chlorpyrifos and 7-10 days in Luna experience will be safer to consumers. This data generated will be useful for regulatory agency for fixing MRLs.
We have synthesized novel chalcogenide glasses from the Se-Te-Sn-Pb system using simple and cost effective met-quench technique. The effect of lead incorporation on micro-hardness and other thermo-mechanical characteristics like volume (V h ) and formation energy (E h ) of micro-voids in the glassy network and modulus of elasticity E of parent Se 78 Te 20 Sn 2 alloy is studied.
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