ABSTRACT This study presents an efficient approach for the separation and preconcentration of norepinephrine (NOR) from pharmaceutical formulations, environmental water, and human urine samples using a dispersive micro – solid phase extraction (DμSPE) technique employing magnetic nanoadsorbents. Two adsorbents, Fe3O4@TTAB and Fe3 O4@SiO2@TTAB, were prepared by functionalising iron oxide and silicacoated iron oxide nanoparticles with the cationic surfactant tetradecyltrimethylammonium bromide (TTAB). NOR was first converted into a sensitive diazonium dye via reaction with diazotised sulphamethazine and then extracted using mixed ademicelle – hemimicelle magnetic solid-phase extraction, followed by spectrophotometric quantification. Key adsorption parameters, including contact time, adsorbent dosage, solution pH, and reagent concentration, were optimised to elucidate the dye adsorption mechanism, and sorbent reusability was evaluated over six adsorption – desorption cycles. The surfactant-coated nanoparticles provided high extraction efficiencies, achieving preconcentration factors of 35 for Fe3O4@TTAB and 56 for Fe3O4@SiO2@TTAB, with recoveries of 96–102% and relative standard deviations below 3% for both adsorbents. The method displayed linearity ranges of 0.1–6.0 μg/mL for Fe3O4@TTAB and 0.05–6.0 μg/ mL for Fe3O4@SiO2@TTAB, with detection limits of 0.035 and 0.019 μg/mL, respectively. These results confirm that DμSPE is a reliable and sustainable approach for NOR extraction and preconcentration from diverse matrices.
Two simple, rapid, and useful spectrophotometric methods were suggest or the determination of sulphadimidine sodium (SDMS) with and without using cloud point extraction technique in pure form and pharmaceutical preparation. The first method was based on diazotization of the Sulphdimidine Sodium drug by sodium nitrite at 5 ºC, followed by coupling with α –Naphthol in basic medium to form an orange colored product . The product was stabilized and its absorption was measured at 473 nm. Beer’s law was obeyed in the concentration range of (1-12) μg∙ml-1. Sandell’s sensitivity was 0.03012 μg∙cm-1, the detection limit was 0.0277 μg∙ml-1, and the limit of Quantitation was 0.03605μg
... Show MoreIn this paper, two types of iron oxide nanomaterial (Fe3O4) and nanocomposite (T-Fe3O4) were created from the bio-waste mass of tangerine peel. These two materials were utilized for adsorption tests to remove cefixime (CFX) from an aqueous solution. Before the adsorption application, both adsorbents have been characterized by various characterizations such as XRD, FTIR, VSM, TEM, and FESEM. The mesoporous nano-crystalline structure of Fe3O4 and T-Fe3O4 nanocomposite with less than 100-nm diameter is confirmed. The adsorption of the obtained adsorbents was evaluated for CFX removal by adjusting several operation parameters to optimize the removal. The optimal conditions for CFX removal were found to be an initial concentration of 40 and 50 m
... Show MoreNanofluid treatment of oil reservoirs is being developed to enhance oil recovery and increase residual trapping capacities of CO2 at the reservoir scale. Recent studies have demonstrated good potential for silica nanoparticles for enhanced oil recovery (EOR) at ambient conditions. Nanofluid composition and exposure time have shown significant effects on the efficiency of EOR. However, there is a serious lack of information regarding the influence of temperature on nanofluid performance; thus the effects of temperature, exposure time and particle size on wettability alteration of oil-wet calcite surface were comprehensively investigated; moreover, the stability of the nanofluids was examined. We found that nanofluid treatment is more efficie
... Show MoreFerric oxide nanoparticles Fe3O4NPs have been prepared by the coprecipitation method, which were used to functionalize the surface of electrospun nanofibers of polyacrylonitrile to increase their effectiveness in adsorption of Congo red (CR) dye from their aqueous solutions. The effect factors of adsorption were systematically investigated such as adsorbent mass, initial concentration, contact time, temperature, ionic strength and pH. The maximum adsorbed amount of the dye was at 0.003g of adsorbent. The adsorption of dye increased with increasing initial dye concentration and the system reaches to the equilibrium state at 150 min. The adsorbed dye capacity decreases with increasing temperature which indicates to the exothermic nature of ad
... Show MoreHeavy metal ion removal from industrial wastewater treatment systems is still difficult because it contains organic contaminants. In this study, functional composite hydrogels with photo Fenton reaction activity were used to decompose organic contaminants. Fe3O4 Nanoparticle, chitosan (CS), and other materials make up the hydrogel. There are different factors that affected Photo-Fenton activity including (pH, H2O2 conc., temp., and exposure period). Atomic force microscopy was used to examine the morphology of the composite and its average diameter (AFM). After 60 minutes of exposure to UV radiation, CS/ Fe3O4 hydrogel composite had degraded methylene blue (M.B.)
... Show MoreA new, Simple, sensitive and accurate spectrophotometric methods have been developed for the determination of sulfamethoxazole (SMZ) drug in pure and dosage forms. This method based on the reaction of sulfamethoxazole (SMZ) with 1,2-napthoquinone-4-sulphonic acid (NQS) to form Nalkylamono naphthoquinone by replacement of the sulphonate group of the naphthoquinone sulphonic acid by an amino group. The colored chromogen shows absorption maximum at 460 nm. The optimum conditions of condensation reaction forms were investigated by (1) univariable method, by optimizing the effect of experimental variables (different bases, reagent concentration, borax concentration and reaction time), (2) central composite design (CCD) including the effect of
... Show MoreTwo quantitative, environment-friendly and easily monitored assays for Ni (II) and Co (III) ions analysis in different lipstick samples collected from 500-Iraqi dinars stores located in Baghdad were introduced. The study was based on the reaction of nickel (II) ions with dimethylglyoxime (DMG) reagent and the reaction of cobalt (III) ions with 1-nitroso-2-naphthol (NN) reagent to produce colored products. The color change was measured by spectrophotometric method at 565 nm and 430 nm for Ni and Co, respectively, with linear calibration graphs in the concentration range 0.25-100 mg L-1 (Ni) and 0.5-100 mg L-1 (Co) and LOD and LOQ of 0.11 mg L-1 and 0.36 mg L-1 (Ni), and 0.15 mg L-1 an
... Show MoreTwosimple, sensitive,accurate, and precise spectrophotometric methods have been developed for the determination of chlorpromazine – HCl in pure form and pharmaceutical formulation. The first method involved treatment of cited drug with a measured excess of permanganate in acid medium and the unreacted oxidant was measured at 525 nm. The second method involves the reaction of the drug with potassium permanganate in the presence of sodium hydroxide to produce a bluish – green colored manganite which is measurable at 610nm. All the experimental variables affecting the development of the manganite ions were investigatedand conditions were optimized. Working linearity ranges were 5-45 µg.mL-1and 1-20 µg.mL-1 by two methods respectively. Th
... Show MoreA simple, accurate and sensitive spectrophotometric method for the determination of Procaine penicillin (PP) is described. The method is based on charge-transfer reaction of PP with metol (N-methyl-p-hydroxy aniline) in the presence of ferric sulphate to form a purple-water soluble complex ,which is stable and has a maximum absorption at 510 nm .A graph of absorbance versus concentration shows that Beer’s low is obeyed over the concentration range of 3-80 µg /ml of PP (i.e.,3-80 ppm) with a molar absorbativity of 4.945 ×103 L.mol-1.cm-1 ,Sandell sensitivity of 0.1190 µg cm-2 ,a relative error of (-1.57)-2.79 % and a standard deviation of less than 0.59 depending on the concentration of PP.The optimum conditions for full co
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