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ANANBIOANAL - 2010
Pharmaceutical R & D Summit
Method Validation, Uncertainty Analysis and Safety Evaluation
of Meptyldinocap in Grapes Using Liquid Chromatography- Mass
Spectrometry
Sudeb Mandal1
, Saktipada Das1
and Anjan Bhattacharyya2
1Department of Chemistry, Kalyani University, Kalyani, WB, India
2Department of Agricultural Chemicals, Bidhan Chandra Krishi Viswavidyalaya, WB, India
M
eptyldinocap (one isomer of dinocap) is a novel powdery mildew fungicide,
is going to introduce in India by Dow AgroSciences to replace dinocap. An
analytical method for the quantitative determination of meptyldinocap (2,4-DNOPC)
as 2,4 dinitro-octylphenyl (2,4-DNOP) in grapes was developed as well as validated
using liquid chromatography tandem mass spectrometry (LC-MS/MS). The method
comprised of an extraction with an acetone: methanol: 4N HCl (100:10:5, v/v/v)
mixture followed by hydrolytic conversion of parent 2,4-DNOPC to the corresponding
phenol metabolite (2,4-DNOP) and clean up was done by liquid: liquid partition using
ethyl acetate. Final quantization was performed by LC-MS/MS of 2,4-DNOP with
negative electrospray ionization using the gradient elution. The method was validated
at concentrations ranging from 0.025-2 µg/g and the limit of quantification (LOQ) of
meptyldinocap in grape samples was 0.025µg/g. The recovery of meptyldinocap
grapes was found to be 92-94 % spiked at different levels with analyte and the
relative standard deviation for repeatability (RSDr
acceptable (less than 10%). The method was rugged as evident from a low global
uncertainty of measurement at 0.05µg/g. Moreover, the developed and validated
method was used to study its dissipation and residue (at harvest) of meptyldinocap
in grape field ecosystem under Indian tropical climate with a view to ensure human
and environmental safety.
) and reproducibility (RSDR
Biography
Dr. Sudeb Mandal has completed his Ph.D from University of Kalyani and Bidhan
Chandra Krishi Viswavidyalaya. He is a trainee Scientist in India’s leading contract
research and testing organization. He has published more than 4 papers in reputed
international journals.
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ANALBIOANAL-2010
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