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Hollow-Fiber Liquid-Phase Microextraction Followed by Gas Chromatography Flame Ionization Detection for the Determination of Amitraz in Honey and Water Samples

Yamini, Yadollah, Faraji, Mohammad, Ghambarian, Mahnaz
Food analytical methods 2015 v.8 no.3 pp. 758-766
Taguchi method, amitraz, detection limit, flame ionization, honey, ionization, liquid-phase microextraction, mixing, pH, sodium acetate, sodium chloride, solvents
This paper reports a two-phase hollow fiber-protected liquid-phase microextraction (HF-LPME) followed by gas chromatography-flame ionization detection as a simple, fast, low-cost, and sensitive method for the determination of amitraz in honey and water samples. The effect of factors effective on the extraction efficiency of amitraz was studied and optimized. The effect of type of extracting solvent was optimized by the one-variable-at-a-time method. The effect of other factors was optimized using the Taguchi method (an orthogonal array design (OAD)) with OA₁₆(4⁴) matrix. The optimal conditions for HF-LPME procedure were found as 1-undecanol as the extracting solvent, sample pH of 6.0 (adjusted with 0.01 mol/L sodium acetate), stirring rate of 1,000 rpm, and extraction time of 45 min without the addition of NaCl. The figures of merit of the method were evaluated in honey and water matrices. In water matrix, the method was linear in the range of 5–2,500 μg/L with a coefficient of determination (r²) corresponding to 0.9996 and relative standard deviation (RSD%) lower than 11 %. Also, in honey samples, a calibration curve was linear in the range of 20–1,000 μg/L with RSD% of 13.8 % and r² > 0.9901. The enrichment factors were 170 and 75, and the limits of detection (LODs) based on S/N = 3 were 3 and 10 μg/L in water and honey samples, respectively. Finally, applicability of the proposed method was evaluated by extraction and determination of amitraz in some honey and water samples and good recoveries (>90 %) were obtained.