Application of MIL-53(Al) prepared from waste materials for solid-phase microextraction of propranolol followed by corona discharge-ion mobility spectrometry (CD-IMS).

In this study, MIL-53(Al) metal-organic framework was prepared from waste raw materials. A polyethylene terephthalate (PET) plastic bottle was used as the source of terephthalic acid, and an aluminium beverage can was applied as the precursor of aluminium salt. The activated MIL-53(Al) was immobilized onto a stainless steel probe of the ion mobility spectrometer (IMS), and the coated probe was used for solid-phase microextraction of propranolol from biological samples before determination. The effect of the different parameters such as pH, ionic strength, and stirring rate of the sample, extraction time, and temperature was studied on the extraction efficiency of propranolol. The linearity was obtained ranging from 5-200 µg L-1 with a determination coefficient (R2) of 0.9988, and the detection limit was calculated 1.7 µg L-1 in the water sample. The relative standard deviations of the method were in the range of 2.5-12.2 %. Finally, the method was utilized for determination of propranolol in the tablet sample.

Application of hollow fiber membrane mediated with titanium dioxide nanowire/reduced graphene oxide nanocomposite in preconcentration of clotrimazole and tylosin.

In this paper, TiO2 nanowires and TiO2 nanoparticles have been successfully anchored on graphene oxide (GO) nanosheets by a facile one-step hydrothermal method. The synthesized TiO2 NWs/RGO and TiO2 NPs/RGO nanocomposites were characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis. After comparatively studying of the as-made nanocomposites, TiO2 NWs/RGO nanocomposite showed the best adsorbing performance and applied as an attractive efficient sorbent reinforced with microporous hollow fiber membrane through the sol-gel technology. In the following, the selected nanocomposite was utilized for simultaneous preconcentration and determination of clotrimazole and tylosin using high performance liquid chromatography (HPLC)-UV detection, respectively. In order to optimize the extraction conditions through affecting parameters (pH, stirring rate, salt addition, extraction time and volume of donor phase), response surface methodology (RSM) was employed as a powerful statistical technique. Under the optimal conditions, the limit of detection (S/N=3) of proposed HFSPME method, was 0.67 µg L(-1) for clotrimazole and 0.91 µg L(-1) for tylosin with good linear ranges of 1.7-8000.0 µg L(-1) and 4.0-6000.0 µg L(-1). The inter-day and intra-day relative standard deviations (RSD%) at 100 µg L(-1) concentration level were in the ranges of 2.10-3.58% for clotrimazole and 3.45-7.80% for tylosin (n=5), respectively. The proposed microextraction device was extended for determination of ultra trace amounts of target analytes in milk and urine samples with satisfactory results.

Extraction and preconcentration of tylosin from milk samples through functionalized TiO2 nanoparticles reinforced with a hollow fiber membrane as a novel solid/liquid-phase microextraction technique.

The aim of this study was to introduce a novel, simple, and highly sensitive preparation method for determination of tylosin in different milk samples. In the so-called functionalized TiO2 hollow fiber solid/liquid-phase microextraction method, the acceptor phase is functionalized TiO2 nanoparticles that are dispersed in the organic solvent and held in the pores and lumen of a porous polypropylene hollow fiber membrane. An effective functionalization of TiO2 nanoparticles has been done in the presence of aqueous H2 O2 and a mild acidic ambient under UV irradiation. This novel extraction method showed excellent extraction efficiency and a high enrichment factor (540.2) in comparison with conventional hollow fiber liquid-phase microextraction. All the experiments were monitored at λmax = 284 nm using a simple double beam UV-visible spectrophotometer. A Taguchi orthogonal array experimental design with an OA16 (4(5) ) matrix was employed to optimize the factors affecting the efficiency of hollow fiber solid/liquid-phase microextraction such as pH, stirring rate, salt addition, extraction time, and the volume of donor phase. This developed method was successfully applied for the separation and determination of tylosin in milk samples with a linear concentration range of 0.51-7000 µg/L (r(2) = 0.991) and 0.21 µg/L as the limit of detection.

Preconcentration and determination of methyl methacrylate by dispersive liquid-liquid microextraction.

This article describes the preconcentration of methyl methacrylate in produced water by the dispersive liquid-liquid microextraction using extraction solvents lighter than water followed by gas chromatography. In the present experiments, 0.4 mL dispersive solvent (ethanol) containing 15.0 µL extraction solvent (toluene) was rapidly injected into the samples and followed by centrifuging and direct injection into the gas chromatograph equipped with flame ionization detector. The parameters affecting the extraction efficiency were evaluated and optimized including toluene (as extraction solvent), ethanol (as dispersive solvent), 15 µL and 0.4 mL (as the volume of extraction and dispersive solvents, respectively), pH 7, 20% ionic strength, and extraction's temperature and time of 20°C and 10 min, respectively. Under the optimum conditions, the figures of merits were determined to be LOD = 10 µg/L, dynamic range = 20-180 µg/L, RSD = 11% (n = 6). The maximum recovery under the optimized condition was determined to be 79.4%.