Determination of insecticides in honey samples collected from Gümüşhane-Turkiye; Box-Behnken design evaluation of experimental parameters

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Abstract
This study deals with the investigation of cyfluthrin, cypermethrin, deltamethrin, and malathion residues in local honey samples from Gümüşhane, Turkey. The determination was performed with GC/MS-MS method with HP-5MS column under certain conditions: 120 ℃ oven temperature, 250 ℃ injection temperature, 121.9 kPa pressure and 1.2-1.8 mL/min flow rates. The samples were picked from eighteen stations of Gümüşhane. Standard addition method was employed in chromatographic determination. No pesticide detected in samples of fifteen stations, nevertheless, subjected pesticides were determined in samples collected from other three stations. The residue levels varied from 0.18 mg/kg to 9.50 mg/kg at 1.5 mL/min flow rate. The results were also evaluated with Box-Behnken Design (BBD) optimization. Multivariate experimental design (flow rate and station, pesticide type) was employed for constructing quadratic models. Regression analysis showed that the experimental results and the predictive values yielded by model are quite close to each other with determination coefficient (R2) of 0.985.

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