Abstract

DEVELOPMENT OF METHOD AND VALIDATION FOR DETERMINATION OF PESTICIDE RESIDUES IN CHILLI BY GCECD (ELECTRON CAPTURE DETECTOR) AND GC-MS (MASS SPECTROMETER)

Sudeep Mishra,* Neelam Richhariya, Samsul Alam, Lalitesh Kumar Thakur and Phool Kumar Patanjali

Abstract

Study was conducted to validate QuEChERS method for qualitative and quantitative determination of some most frequently used organochlorine pesticides residue levels on chilli by Gas Chromatography. Solid Phase Extraction (SPE) using ethylacetate, anhy. sodium sulphate, magnesium sulphate was used to extract pesticides present in a sample and clean up of interfering pigments was done by Primary Secondary Amine (PSA), Activated charcoal and C18. Instruments GC-ECD (Agilent Technologies) and GC Model 7890A (Agilent Technologies) with mass (5975C inert XL EI/CI MSD) triple axis detector was taken for study. Limit of Detection (LOD) and LOQ (Limit of Quantification) were calculated for specific pesticides against chilli matrix and was found that values are below MRL (Maximum Residue Limit) set by PFA/Codex/EPA and FDA. Recovery studies were carried out at 0.05 mg/kg concentration level with mean recovery falls from 82.67 % to 92.0 % with Relative Standard Deviation (RSD) below 10%. Repeatability and reproducibility of the instrument taken for study as per Codex, EPA and FDA guidelines. Linearity of the instrument were checked and found linear response when calibration curve was plotted between an area of standard mixture against different concentration levels of 0.001, 0.005, 0.05, 0.01, 0.5 and 1.0 mg/kg with regression co-efficient (r2) lies in the range 0.996 to 0.999.

Keywords: Chilli, Pesticides, LOD, LOQ, MRL, QuEChERS.