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.
A new, simple and sensitive spectrophotometric method was described for the determination of famotidine (FAM) as a pure material and in pharmaceutical formulation. This method was based on diazotization and coupling reaction between famotidine and diazotized solution of metochlopramide hydrochloride (DMPH) in the presence of phosphate buffer solution to give a compound of azo dye having orange color soluble in water with high absorptivity at a wave length of 478 nm. The data shows that FAM and DMPH combine in the molar ratio of 1:1 at PH 7.0 .The method obeys Beer's law over concentration range of 1-40 ?g.ml-1 of famotidine with a correlation coefficient of 0.9955 and a detection limit of 0.10 ?g.ml-1. The apparent molar absorptivity re
... Show MoreA robust and sensitive analytical method is presented for the extraction and determination of six pharmaceuticals in freshwater sediments.
A hybrid cadmium sulfide nanoparticles (CdSNPs) electroluminescence (EL) device was fabricated by Phase – Segregated Method and characterized. It was fabricated as layers of (ITO/poly-TPD:CdS ) and (ITO/poly-TPD:CdS /Alq3). Poly-TPD is an excellent Hole Transport Layer (HTL), CdSNPs is an emitting layer and Alq3 as electron transport layer (ETL). The EL of Organic-Inorganic Light Emitting Diode (OILED) was studied at room temperature at 26V. This was achieved according to band-to-band transition in CdSNPs. From the I-V curve behavior, the addition of Alq3 layer decreased the transfer of electrons by about 250 times. The I-V behavior for (poly-TPD/CdS) is exponential with a maximum current of 4500 µA. While, the current i
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Naproxen(NPX) imprinted liquid electrodes of polymers are built using polymerization precipitation. The molecularly imprinted (MIP) and non imprinted (NIP) polymers were synthesized using NPX as a template. In the polymerization precipitation involved, styrene(STY) was used as monomer, N,N-methylenediacrylamide (N,N-MDAM) as a cross-linker and benzoyl peroxide (BPO) as an initiator. The molecularly imprinted membranes and the non-imprinted membranes were prepared using acetophenone(AOPH) and di octylphathalate(DOP)as plasticizers in PVC matrix. The slopes and detection limits of the liquid electrodes ranged from)-18.1,-17.72 (mV/decade and )4.0 x 10-
... Show MoreTow simple, rapid and sensitive spectrophotometric methods for the determination of mesalazine in pharmaceutical preparations have been carried out. The proposed methods depend on oxidative coupling reaction of mesalazine with m-aminophenol in the existence of N-bromosuccinamide in alkaline medium (method A) and 2,6-dihydroxybenzoic acid in the existence of sodium metaperiodate in basic medium (method B) to produce colored products , show highest absorptions at 640 (nm) and 515 (nm), alternately. Beer’s law was consistent in concentrations extent of 1.25-30 and 0.5-12.5 (µg.mL-1) with molar absorptivity of 0.36×104 and 0.77×104 L.mol-1.cm<
... Show MoreA procedure, depending on the derivatization and determination of aniline was depicted andvalidated in this study. 8-hydroxyquinoline (8-HQ) was used as the derivatizing agent for thedetermination of aniline. An optimization study was performed for the derivatization reaction, i.e.,the diazonium coupling reaction, the optimum parameters were as follows: 22 mM of hydrochloricacid, 54mM of sodium hydroxide, and 1.8mM of sodium nitrate. The optimization study of themethod of cloud point extraction (CPE) revealed that the extraction solvent was 0.5 ml of Triton X-100, the optimum temperature was 90 °C, and the incubation time was 25 min. The linearity,correlation coefficients, molar absorptivities, and limits of detection were improved using t
... Show MoreChromium tanned leather wastes (CTLW) and vegetable tanned leather wastes (VTLW) were used as adsorbent materials to remove the Biebrich scarlet dye (BS), as an anionic dye from wastewater, using an adsorption method. The effects of various factors, such as weight of leather waste, time of shaking, and the starting concentration of Biebrich scarlet dye, temperature and pH were studied. It described the adsorption process using Langmuir and Freundlich isotherm models. The obtained results agreed well with the Langmuir model, and the maximum adsorption capacities of CTLW and VTLW were 73.5294 and 78.1250 mg.g⁻¹, respectively, suggesting a monolayer adsorption process. The adsorption kinetic was found to follow a pseudo-second-order kinetic
... Show MoreSn(II) complex of the type, [Sn(SMZ)2]Cl2 was synthesized by the interaction of Sulfamethoxazole ligand and Tin Chloride, the complex was confirmed on the basis of results of elemental analyses, FT-IR, UV-Vis, molar conductance (Ëm). The elemental analysis data, suggests the stoichiometry to be 1:2 (metal: ligand) and determination of the formula of a coordination a complex formed between the Sn(II) ion and the SMZ using Job’s method of continuous variations. The study of (Ëm), indicated the electrolytic nature type 1:2. The [Sn(SMZ)2]Cl2 was screened for antibacterial activity against Gram-ve (Escherichia coli and Gram+ve (Staphylococcus aureus) and (Candida albicans) antifungal. The IR spectral data suggested that the coordination sit
... Show MoreThe determination of critical micelle concentration of selected non-ionic surfactants (Tween 20,40 and 80) have been investigated using magnetic water(MW)as an aqueous medium.Conductometry technique is used to determine critical micelle concentration.The effect of alcohol addition and temperature variation at the range(293.15 -303.15K) are also pursued. It is concluded that the process of micellization is spontaneous and endothermic because of the observed free energy of micellization (ΔGom) , enthalpy change of micellization (ΔHom), and entropy change of micellization (ΔSom) for the system was also studied.The properties of the non-ionic surfactants were studied, both in absence and presence of
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