Modification of AOAC Multiresidue Method for Determination of Synthetic Pyrethroid Residues in Fruits, Vegetables, and Grains. Part I: Acetonitrile Extraction System and Optimization of Florisil Cleanup and Gas Chromatography

We present a multiresidue method for determination of synthetic pyrethroids in fruits, vegetables, and grains. The method is a modification of AOAC Method 970.52. Residues are extracted with acetonitrile (for fruits and vegetables) or acetonitrile–water (2 + 1) (for grains) and then transferred to hexane. Coextractives are removed by acetonitrile partitioning and open-column chromatography with deactivated Florisil. The final extract is analyzed by gas chromatography with electron capture detection (GC–ECD). An HP-17 wide-bore column is used to determine the total isomeric content of each insecticide, and a DB-5 narrow-bore column is used to determine the individual isomeric contents of each insecticide. The method was used to recover 8 pyrethroids (biphenthrin, fenpropathrin, cyhalothrin, permethrin, cypermethrin, fluvalinate, fenvalerate, and deltamethrin) spiked at 0.01–4.0 mg/kg in 20 crops (apple, pear, peach, banana, grape, strawberry, potato, tomato, cucumber, pepper, cabbage, carrot, celery, polished rice, wheat, green gram, buckwheat, sorghum, maize, and barley). Recoveries of the 8 pyrethroid insecticides in 6 crops ranged from 83.8 to 112.8%, with a coefficient of variation (CV) of 2.00 to 12.09% for the narrow- bore capillary GC (n = 6) and from 82.8 to 106.4%, CV = 2.93–12.19%, for the wide-bore capillary GC (n = 6). The minimum detectable levels of 0.004–0.028 mg/kg (for fruits and vegetables) or 0.01–0.08 mg/kg (for grains) for the 8 pyrethroids are easy to detect.