Synthesis and application of molecularly imprinted nanoparticles combined ultrasonic assisted for highly selective solid phase extraction trace amount of celecoxib from human plasma samples using design expert (DXB) software

In this work molecular imprinted nanoparticles (MINPs) was synthesized and applied for ultrasonic assisted solid phase extraction of celecoxib (CEL) from human plasma sample following its combination by HPLC–UV. The MINPs were prepared in a non-covalent approach using methacrylic acid as monomer, CEL as template, ethylene glycol dimethacrylate as cross-linker, and 2,2-azobisisobutyronitrile (AIBN) as the initiator of polymerization. pH, volume of rinsing and eluent solvent and amount of sorbent influence on response were investigated using factorial experimental design, while optimum point was achieved and set as 250 mg sorbent, pH 7.0, 1.5 mL washing solvent and 2 mL eluent by analysis of results according to design expert (DX) software. At above specified conditions, CEL in human plasma with complicated matrices with acceptable high recoveries (96%) and RSD% lower than 10% was quantified and estimated.The proposed MISPE-HPLC–UV method has linear responses among peak area and concentrations of CEL in the range of 0.2–2000 μg L⁻¹, with regression coefficient of 0.98. The limit of detection (LOD) and quantification (LOQ) based on three and ten times of the noise of HPLC peaks correspond to blank solution were 0.08 and 0.18 μg L⁻¹, respectively.     

Application of Graphene as a Sorbent for Simultaneous Preconcentration and Determination of Trace Amounts of Cobalt and Nickel in Environmental Water and Vegetable Samples

A new method using a column packed with graphene as adsorbent was developed for the preconcentration of trace amounts of cobalt (Co) and nickel (Ni) prior to their determinations by flame atomic absorption spectrometry. Several factors influencing the extraction efficiency of Co and Ni and their subsequent determinations, such as pH, amounts of the chelating agent, flow rates of sample and eluent solution, eluent type and its volume, breakthrough volume, and adsorption capacity were established. Under the optimum conditions, the calibration graphs were linear in the range of 4.0‐200.0 μg L^?1 and 5.0‐200.0 μg L^?1 with detection limits of 0.36 μg L^?1 and 0.51 μg L^?1 for Co and Ni, respectively. Good relative standard deviations for ten determinations of 100.0 μg L^?1 of Co and Ni were 3.2 and 3.6%, respectively. The results for determination of Co and Ni in tap water, river water, sea water, vegetable and spiked samples have demonstrated the accuracy and applicability of the proposed method. To validate the proposed method, three certified reference materials of environment water (GSBZ 50030‐94 and GSB 07‐1186‐2000) and tomato leaf (GSBZ 51001‐94) were analyzed, and the determined values were in good agreement with the certified values.     

Membrane-based microchannel device for continuous quantitative extraction of dissolved free sulfide from water and from oil

Underground fluids are important natural sources of drinking water, geothermal energy, and oil-based fuels. To facilitate the surveying of such underground fluids, a novel microchannel extraction device was investigated for in-line continuous analysis and flow injection analysis of sulfide levels in water and in oil. Of the four designs investigated, the honeycomb-patterned microchannel extraction (HMCE) device was found to offer the most effective liquid–liquid extraction. In the HMCE device, a thin silicone membrane was sandwiched between two polydimethylsiloxane plates in which honeycomb-patterned microchannels had been fabricated. The identical patterns on the two plates were accurately aligned. The extracted sulfide was detected by quenching monitoring of fluorescein mercuric acetate (FMA). The sulfide extraction efficiencies from water and oil samples of the HMCE device and of three other designs (two annular and one rectangular channel) were examined theoretically and experimentally. The best performance was obtained with the HMCE device because of its thin sample layer (small diffusion distance) and large interface area. Quantitative extraction from both water and oil could be obtained using the HMCE device. The estimated limit of detection for continuous monitoring was 0.05 μM, and sulfide concentrations in the range of 0.15–10 μM could be determined when the acceptor was 5 μM FMA alkaline solution. The method was applied to natural water analysis using flow injection mode, and the data agreed with those obtained using headspace gas chromatography-flame photometric detection. The analysis of hydrogen sulfide levels in prepared oil samples was also performed. The proposed device is expected to be used for real time survey of oil wells and groundwater wells.     

Spectrophotometry Determination Of Boron With 4-(P-Sulfophenylazo)-1, 8-Dihydroxynaphthalene

Abstract

4-(p-Sulfophenylazo)-l, 8-dihydroxynaphthalene (SPADN) was synthesized to study as a new reagent for the spectro-photometric determination of boron, measuring its absorbance on addition of boron present as boric acid at pH 8.6. The procedure involved mixing aliquots of the sample, ammonium buffer, EDTA and SPADN solutions. Various exchange equilibrium constants in the ion-association extraction systems of SPADN with zephiramine were also determined.     

Degradation effects in the extraction of antioxidants from birch bark using water at elevated temperature and pressure

Experiments with birch bark samples have been carried to enable a distinction between extraction and degradation effects during pressurised hot water extraction. Two samples, E80 and E180, contained birch bark extracts obtained after extraction at 80 and 180 °C for up to 45 min, respectively. Two other samples, P80 and P180, were only extracted for 5 min at the two temperatures and were thereafter filtered and hydrothermally treated at 80 and 180 °C, respectively. During the latter treatment, samples were collected at different times to assess the stability of the extracted compounds. An offline DPPH (2,2-diphenyl-1-picrylhydrazyl) assay, as well as a high performance liquid chromatographic separation coupled to an electrochemical detector, were used to determine the antioxidant capacity of the processed samples. The results obtained with the different techniques were compared to assess the yield of the extraction and degradation processes. In addition, an online hyphenated system comprising high performance liquid chromatography coupled to diode-array; electrochemical; and tandem mass spectrometric detection (HPLC-DAD-ECD-MS/MS) was used to study the compositions of the extracts in more detail. The results for the samples processed at 80 °C showed that the extraction reached a steady-state already after 5 min, and that the extracted compounds were stable throughout the entire extraction process. Processing at 180 °C, on the other hand, gave rise to partly degraded extracts with a multitude of peaks in both the diode array and electrochemical detectors, and a higher antioxidant capacity compared to for the extracts obtained at 80 °C. It is concluded that HPLC-DAD-ECD is a more appropriate technique for the determination of antioxidants than the DPPH assay. The mass spectrometric results indicate that one of the extracted antioxidants, catechin, was isomerised to its diastereoisomers; (+)-catechin, (−)-catechin, (+)-epicatechin, and (−)-epicatechin.     

Cost‐efficient magnetic nanoporous carbon derived from citrus peel for the selective adsorption of seven insecticides

A magnetic solid‐phase extraction adsorbent that consisted of citrus peel‐derived nanoporous carbon and silica‐coated Fe₃O₄ microspheres (C/SiO₂@Fe₃O₄) was successfully fabricated by co‐precipitation. As a modifier for magnetic microspheres, citrus peel‐derived nanoporous carbon was not only economical and renewable for its raw material, but exerted enormous nanosized pore structure, which could directly influence the type of adsorbed analytes. The C/SiO₂@Fe₃O₄ also possessed the advantages of Fe₃O₄ microspheres like superparamagnetism, which could be easily separated magnetically after adsorption. Integrating the superior of biomass‐derived nanoporous carbon and Fe₃O₄ microspheres, the as‐prepared C/SiO₂@Fe₃O₄ showed high extraction efficiency for target analytes. The obtained material was characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, X‐ray photoelectron spectroscopy, and the Brunauer–Emmett–Teller method, which demonstrated that C/SiO₂@Fe₃O₄ was successfully synthesized. Under the optimal conditions, the adsorbent was selected for the selective adsorption of seven insecticides before gas chromatography with mass spectrometry detection, and good linearity was obtained in the concentration range of 2–200 μg/kg with the correlation coefficient ranging from 0.9952 to 0.9997. The limits of detection were in the range of 0.03–0.39 μg/kg. The proposed method has been successfully applied to the enrichment and detection of seven insecticides in real vegetable samples.     

Ultrasound-assisted extraction of antimony and cobalt from inorganic environmental samples using a cup-horn sonoreactor prior to their determination by electrothermal-atomic absorption spectrometry

A simple, fast and reliable method is described for the quantitative extraction of Sb and Co from inorganic environmental matrices containing variable amounts of silicates prior to their determination by electrothermal-atomic absorption spectrometry. The method is based on the ultrasound-assisted extraction of both elements using the mixture 20% v/v HF + 20% v/v HNO₃ as extractant. The extraction procedure was carried out in closed Eppendorf vials immersed in a cup-horn sonoreactor for 20?min. Once extraction has been accomplished, the supernatant liquid is separated from the solid phase and subsequently transferred into the autosampler of the instrument. A two-level full factorial design (2⁴) was applied for screening optimisation of the variables influencing the ultrasonic extraction. These variables were: sonication time; amplitude of the ultrasound energy; nitric and hydrofluoric acid concentrations. MLDs were 0.20 and 0.06?µg?·?g^?1 for Sb and Co, respectively. Between-batch precision values, expressed as relative standard deviations (n?=?3), were less than 5.5 and 9.6% for Sb and Co, respectively. The method was evaluated using a wide variety of inorganic certified reference materials, such as SRM 2702 (Marine Sediment), SRM 2782 (Industrial Sludge), BCR 176R (Fly Ash), SRM 1633b (Coal Fly Ash) SRM 2710 (Montana Soil) and SRM 2711 (Montana Soil).     

Extraction of Gallium (III) with O,O, S-Triethyldithiophosphate

Abstract

A method is presented for the rapid solvent extraction of gallium (III) with o, o, s-triethyldithiophosphate. Quantitative extraction results from 4–9 M hydrochloric acid, using 100% extractant. The extract-able species is H[GaCl₄]·2(C₂H₅ O₂)₂ P(S)SC₂H₅.     

Optical multiresolution analysis with spatial localization

Multiresolution analysis is very useful for characterization of textures, segmentation tasks, and feature enhancement. The development of optical methods to perform such procedures is highly promissory for real-time applications. Usually, the optical implementations of multiresolution analysis consist in the decomposition of the input scene in different frequency bands, obtaining various filtered versions of the scene. However, under certain circumstances it could be useful to provide just one version of the scene where the different filters are applied in different regions. This procedure could be specially interesting for biological and medical applications in situations when the approximate localization of the scale information is known a priori. In this paper we present a fully optical method to perform multiresolution analysis with spatial localization. By means of the proposed technique, the multi-scale analysis is performed at once in a unique image. The experimental set-up consist of a double-pass convergent optical processor. The first stage of the device allows the multiple band decomposition, while the second stage confines the information of each band to different regions of the object and recombines it to achieve the desired operation. Numerical simulations and experimental results, which prove the very good performance of the method, are presented.