An environment-friendly and rapid liquid-liquid microextraction based on new synthesized hydrophobic deep eutectic solvent for separation and preconcentration of erythrosine (E127) in biological and pharmaceutical samples.

In this study, a new deep eutectic solvent (DES) consist of tetrabuthylammonium bromide (TBABr) and 1-octanol at 1:2 M ratio was prepared for the first time and characterized by Fourier transform infrared spectroscopy (FT-IR), proton nuclear magnetic resonance (1H NMR) and carbon nuclear magnetic resonance (13C NMR) techniques. The new DES was used as an extraction solvent in the ultrasound assisted liquid-liquid microextraction (UA-LLME) of Erythrosine (E127) in blood, urine, pharmaceutical tablet and syrup samples. Accurate and sensitive determination of erythrosine was accomplished with the combination use of DES-UA-LLME and UV-Vis spectrophotometric detection. Before applying UA-LLME, while protein precipitation was applied to blood samples, pharmaceutical tablets were homogenized and dissolved in methanol. The proposed DES-UA-LLME/UV-VIS procedure was applied directly to urine, syrup sample and supernatant of blood and tablet samples with high recoveries in range of 90% and 100%. Erythrosine in the aqueous sample phase was extracted into 200 µL hydrophobic DES phase at pH 7.0. The effect of important analytical variables such as pH of sample solution, mol ratio of DES components, volume of DES, ultrasonic-based extraction time, sample volume and salt effect were optimized. The preconcentration factor (PF), limit of detection (LOD), intra-day and inter-day relative standard deviations (RSD, %) for the developed procedure were found as 40, 3.75 µg·L-1, 2.6% and 4.6%, respectively.

TiO2 nanoparticles and C-Nanofibers modified magnetic Fe3O4 nanospheres (TiO2@Fe3O4@C-NF): A multifunctional hybrid material for magnetic solid-phase extraction of ibuprofen and photocatalytic degradation of drug molecules and azo dye.

Accurate sensitive analysis of drug ingredient substances in biological, pharmaceutical and environmental samples and removal of drug ingredient substances in environmental samples owngreat importance for sustaining viability. The realization of these processes using a single material offers significant advantages in terms of cost, time and ease of use. In this study, TiO2 nanoparticles and C-Nanofibers modified magnetic Fe3O4 nanospheres (TiO2@Fe3O4@C-NFs) synthesized as a multifunctional material employing a simple hydrothermal synthesis method. This innovative material was exploited in the magnetic solid-phase extraction (MSPE) method for the preconcentration of ibuprofen and photocatalytic degradation of antibiotics, non-steroidal anti-inflammatory drugs (NSAIDs), and azo dye. To our knowledge, no studies have been previously conducted using the same material as magnetic solid-phase extraction adsorbent and magnetically separable photocatalyst. The characterization of TiO2@Fe3O4@C-NFs was carried out by XRD, FE-SEM, EDX and Raman techniques. The main analytical parameters affecting MSPE performance of ibuprofen such as pH, sorbent amount eluent type and volume and sample volume were optimized. The optimum values of the method were determined at the following parameters: pH 4.0, adsorbent amount 150 mg and eluent 2 mL of acetone. Ibuprofen analysis after MSPE was carried out using a high-performance liquid chromatography diode array detection system (HPLC-DAD). The photocatalytic degradation efficiencies of TiO2@Fe3O4@C-NF hybrid material for probe-analytes reached 80-100% and the complete degradation attained within the range of 8-125 min under UV irradiation. Simple preparation, practical isolation from solutions, high efficiency, reproducibility, and sustainability are the main advantages of the TiO2@Fe3O4@C-NFs for MSPE and photocatalytic degradation applications.

Green synthesis of magnetic carbon nanodot/graphene oxide hybrid material (Fe3O4@C-nanodot@GO) for magnetic solid phase extraction of ibuprofen in human blood samples prior to HPLC-DAD determination.

In this study, a green production method was used to obtain magnetic carbon nanodot/graphene oxide hybrid material (Fe3O4@C-nanodot@GO) for the magnetic solid phase extraction (MSPE) of ibuprofen (IBU) in human plasma prior to HPLC-DAD determination. For the first time in the literature, Fe3O4@C-nanodot@GO hybrid material was synthesized and used as an adsorbent. C-nanodots were produced from pasteurized cow milk by using a simple and cheap hydrothermal method. After production of the C-nanodots and GO, Fe3O4@C-nanodot@GO hybrid material was fabricated in green solvent medium by using an one-step hydrothermal method. The method was based on the simple separation, preconcentration and analysis of ibuprofen by using MSPE-HPLC-DAD combination. The concentration changes of ibuprofen in human bloods against time were successfully monitored by using this combined method. For this purpose, blood samples were taken from volunteers at certain intervals after the administration of a certain dose of ibuprofen, and the MSPE method was used to monitor the concentration changes of ibuprofen in the blood samples. Experimental variables affecting the extraction efficiency of IBU such as sample solution pH, amount of adsorbent, extraction time, eluent type and volume were studied and optimized in the details. The characterization studies for the Fe3O4@C-nanodot@GO were carried out by X-ray diffraction spectrometry (XRD), Fourier transform infrared spectrometry (FT-IR), Raman spectrometry (Raman), energy dispersive x-ray (EDX), vibrating sample magnetometry (VSM) and scanning electron microscopy (SEM) techniques. Under the optimum experimental conditions, the limit of detection (LOD) was 8.0 ng mL-1 and the recoveries at three spiked levels in human plasma were ranged from 91.0% to 95.0% with the relative standard deviation (RSD %) less than 4.0 % (n = 6). The results show that together use of MSPE with HPLC-DAD provides a simple and rapid analysis of ibuprofen in human plasma samples.