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In this study, the performances of four ionic-liquid-based microextraction methods, ionic-liquid-based dispersive liquid-liquid microextraction (IL-DLLME), ionic-liquid-based ultrasound-assisted emulsification microextraction (IL-USA-ME), temperature-controlled ionic-liquid dispersive liquid-phase microextraction (TC-IL-DLME), and ultrasound-assisted temperature-controlled ionic-liquid dispersive liquid-phase microextraction (USA-TC-IL-DLME), were investigated for extraction of three bioactive compounds (anethole, estragole, and anisaldehyde) from different plant extracts and human urine. Anethole and estragole were chosen because they can alter cellular processes positively or negatively, and an efficient method is needed for their extraction and sensitive determination in the samples mentioned. Because there is no previous report on the separation of anethole and estragole (structural isomers), first, simultaneous gradient elution and flow programming were used. The microextraction methods were then applied and compared for analysis of these compounds in plant extracts and human urine by use of high-performance liquid chromatography (HPLC). The effect of conditions on extraction efficiency was studied and under the optimum conditions, the best enrichment factors (58-64), limits of detection (14-18 ng mL(-1)), limits of quantification (47-60 ng mL(-1)), and recovery (94.4-101.7 %) were obtained by use of USA-TC-IL-DLME. The optimized conditions were used to determine anethole, estragole, and para-anisaldehyde in fennel, anise, and tarragon extracts and in human urine.

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In the present study, hybrid amine-functionalized titania/silica nanoparticles were employed as a new and novel adsorbent for solid-phase extraction of Pb 2+ , Cu 2+ , and Zn 2+ ions prior to their determination using flame atomic absorption spectrometry. Under the best conditions (including adsorbent, 0.4 g; eluent, 5.0 mL nitric acid (HNO 3 ), 3.0 mol L −1 , 1.0 mL min −1 ; and sample, pH 5.0, 3.0 mL min −1 ), detection limits, adsorption capacities, and preconcentration factors were 0.12-0.24 μg L −1 , 7.1-20.7 mg g −1 , and 200, respectively. To predict the adsorption isotherms, different isotherm models were studied and the obtained results showed that the Langmuir model is the most suitable one to explain the experimental data. The kinetics of the reaction followed pseudosecond-order kinetic model. Thermodynamic parameters like free energy (ΔG 0 ) and enthalpy (ΔH 0 ) confirmed the spontaneous and exothermic nature of the process. The method was successfully applied for determination of the analytes in different food and water samples.