A rapid and simple sample preparation method was developed for simultaneous determination of three triazine herbicides in honey samples. The selected herbicides were extracted from honey samples by ionic liquid dispersive liquid-liquid microextraction, separated on a C column (250 mm × 4.6 mm id, 5 μm) using acetonitrile and H O as the mobile phase with gradient elution, and then detected by high-performance liquid chromatography. The parameters, such as the type and volume of the extraction and disperser solvent, ion strength, pH, extraction time, and centrifuge time were optimized in order to provide the excellent extraction performance. Good linearity was showed for all the target herbicides over the tested concentration range with correlation coefficient higher than 0.994. Three spiked levels (0.005, 0.05, 0.10 mg/kg) were applied for determination of the recoveries of the targets in honey samples in the range of 80-103% with relative standard deviations not larger than 10.6%. The limits of quantification for the analytes ranged between 1.5 and 4.0 μg/kg. The developed method was applied for determination of the target compounds residues in real samples.
An aqueous biphasic system based on cholinium propanoate and phosphate solution was developed for the fast extraction and determination of bisphenol A in honey samples. The phase diagrams of the aqueous biphasic systems with cholinium propanoate (ionic liquid) and phosphate solutions were investigated, and the biphasic regions of the aqueous biphasic systems decreased with the increase of pH values of the phosphate solutions. The aqueous biphasic system was applied for the analyte extraction. After extraction, the analyte was separated on a C18 column (150 mm × 2.1 mm i. d., 5 μm) using acetonitrile and ammonium acetate as the mobile phase. The parameters, such as the conductivity and viscosity of the ionic liquid solutions, pH values of the phosphate solutions, and extraction efficiency were optimized to achieve the excellent extraction performance. Good linearity was shown for the analyte over the tested concentration range (0.01–10.0 mg/kg) with correlation coefficient higher than 0.991. Three spiked levels (0.01, 0.05, 0.10 mg/kg) were applied for determination of the recoveries of the analyte in honey samples in the range of 78–112% with relative standard deviations of 5.5–10.2%. The limit of detection and limit of quantification for the analyte were 0.003 and 0.01 mg/kg, respectively. The developed method was applied for the determination of the analyte in real samples with high sensitivity.
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