Journal :   Asian Journal of Research in Chemistry

Volume No. :   9

Issue No. :  1

Year :  2016

Pages :   13-21

ISSN Print :  0974-4169

ISSN Online :  0974-4150


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Method Development and Validation of Multiclass Pesticide Residues and Metabolites in Wheat by GC-ECD and GC-MS



Address:   Mahesh K. Saini, Sudeep Mishra, Samsul Alam*, Lalitesh K. Thakur, Ompal Singh, Syed K. Raza
Institute of Pesticide Formulation Technology, Sector-20, Udyog Vihar, Opp. Ambience Mall, NH-8, Gurgaon, Haryana-122016, India
*Corresponding Author
DOI No: 10.5958/0974-4150.2016.00003.1

ABSTRACT:
A method was developed and validated for analysis of 25 multiclass pesticide residues and their metabolites in wheat grains using GC-ECD for quantification, and GC-MS for confirmation. Samples were treated through a method developed by slight modification in QuEChERS technique. The GC-ECD instrument was calibrated at 6 calibration levels (viz. 0.005, 0.010, 0.050, 0.100,0.250, 0.500 mg/Kg) with regression co-efficient (r2) varying from 0.9993 to 0.9756. Sample preparation include extraction by Acetonitrile solvent (HPLC grade) and clean up by C-18, PSA and anhydrous MgSO4. Limit of Detection (LOD) of pesticides in wheat matrix varies from 0.002-0.06µg/g and Limit of Quantitation (LOQ)from 0.004 to 0.2µg/g. Mean recovery percentage of pesticides at 1 LOQ lies in range of 79.77-128.04 with RSD below 16.35%. Uncertainty measured at three sources–purity of standards, weighing and instrument precision. Maximum expanded uncertainty (2U) falls between the range of 0.0008–0.487.
KEYWORDS:
Pesticide residue; Method development; LOD; LOQ; Wheat.
Cite:
Mahesh K. Saini, Sudeep Mishra, Samsul Alam, Lalitesh K. Thakur, Ompal Singh, Syed K. Raza. Method Development and Validation of Multiclass Pesticide Residues and Metabolites in Wheat by GC-ECD and GC-MS. Asian J. Research Chem. 9(1): Jan., 2016; Page 13-21.
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