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Asian Journal of Research in Chemistry
Year : 2016, Volume : 9, Issue : 1
First page : ( 13) Last page : ( 21)
Print ISSN : 0974-4169. Online ISSN : 0974-4150.
Article DOI : 10.5958/0974-4150.2016.00003.1

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

Saini Mahesh K., Mishra Sudeep, Alam Samsul*, Thakur Lalitesh K., Singh Ompal, Raza Syed K.

Institute of Pesticide Formulation Technology, Sector-20, Udyog Vihar, Opp. Ambience Mall, NH-8, Gurgaon, Haryana-122016, India

*Corresponding Author E-mail: alam_samsul@rediffmail.com

Online published on 9 March, 2016.

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.

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Keywords

Pesticide residue, Method development, LOD, LOQ, Wheat.

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