A simple HPLC method for determination of permethrin residues in wine

Abstract

An isocratic High Performance Liquid Chromatographic (HPLC) method was optimized for 3-phenoxybenzyl (1RS)-cis-trans-3-(2,2-dichlorovinyl)-2,2-dimethyl-cyclopropanecarboxylate (permethrin) residues identification and quantification in wine matrix. Analytical reverse phase (RP) C-18 column was used (25 cm × 4 mm i.d., 5 μ m) with mobile phase consisting of acetonitrile and water in ratio 70 %/30 % (v v⁻¹), flow-rate 2.0 mL min⁻¹, UV-detection at 215 nm and controlled oven temperature at 25°C. The peaks of isomers were identified with the retention times as compared to standard cis-/trans- mixture and confirmed with characteristic spectra using photodiode array detector. Under these conditions, permethrin isomers were well separated with resolution 2.8 and no interference with the naturally present wine compounds was observed. The method was validated for linearity, precision, accuracy, limit of detection (LOD) and limit of quantification (LOQ). Linear regression analysis data proved a good linear relationship (correlation coefficients, r², for cis- and trans-isomer are: 0.9995 and 0.9997, respectively) between response of the detector and concentration of permethrin isomers over a wide concentration range for both isomers (0.55 mg L⁻¹ −4.40 mg L⁻¹). Experimental data showed mean recoveries between 93.95% and 96.58% with RSD values in range: 0.89% −3.69%. The effect of ethanol content in the solvent on permethrin isomers peak areas was also studied and 60% v v⁻¹ ethanol was found to be optimal for sample preparation. The method was successfully tested on 20 commercial wine samples from the market in which no permethrin was detected. Thus, it was proved that it is suitable for routine permethrin residues analysis. The proposed method is suitable for routine analysis because of the simple sample preparation, acceptable run-time, low cost and its applicability with conventional instruments.

Keywords:

• Permethrin
• residues
• wine
• HPLC

Notes

*The values correspond to % in correlation with target permethrin quantity (2 mg L^{− 1} is taken as 100 %, wt wt^{− 1}).

**RSD: Relative standard deviation.

*sum: Result for summa of isomers.