Multiresidue Gas Chromatographic Method for Determining Synthetic Pyrethroid Pesticides in Agricultural Products: Collaborative Study

Abstract

Fourteen laboratories from 6 countries and regions participated in an international collaborative study to evaluate a multiresidue gas chromatographic (GC) method for determining 8 synthetic pyrethroid pesticides in grains, fruits, and vegetables. The study design was based on Youden's matched-pairs principle for collaborative tests of analytical methods. Each laboratory analyzed 12 collaborative samples of wheat, oranges, and tomatoes as blind samples. Wheat samples were extracted with acetonitrile-water (2 + 1), while orange and tomato samples were extracted with acetone. Residues were partitioned into hexane, evaporated to dryness with a rotary evaporator, and then dissolved in hexane. The hexane extract was partitioned with acetonitrile and cleaned up on a 5% water-deactivated Florisil column with 6% ethyl ether in hexane as eluant. Residue concentrations were determined by GC with electron capture detection with splitless injection by comparison with single-point calibration standards. The appropriate standard concentration was determined by screening sample extracts before analysis. The multiresidue method was tested over the concentration range of 0.095-1.909 mg/kg depending on the 8 different of pesticides and agricultural products analyzed in the collaborative study. Statistical analysis of data from 13 laboratories showed weighted average recoveries for 8 pyrethroids in wheat, oranges, and tomatoes at 0.105-1.909, 0.095-1.909, and 0.105-0.954 mg/kg, respectively, ranging from 91.8 to 100.2%, from 88.1 to 100.6%, and from 88.2 to 101.5%, respectively. Reproducibility relative standard deviation values ranged from 6.46 to 17.74%, from 5.94 to 18.13%, and from 5.59 to 10.48%, respectively. Repeatability relative standard deviation values ranged from 6.34 to 10.84%, from 5.19 to 11.72%, and from 3.20 to 8.09%, respectively. The multiresidue GC method for determining synthetic pyrethroid pesticides in agricultural products has been adopted first action by AOAC INTERNATIONAL.