An electrochemical sensor based on manganese dioxide nanorodMnO2and Graphene oxide (GO) functionalized with 4-amino, 3-substituted 1H, 1, 2, 4 Triazole 5(4H) thion (FGO)/MnO2Nanocompositewas developed for voltammetric determination of Tetracycline (TET).The working electrode WE of SPCE was modified bya drop casting method. X-ray powder diffractometer (XRD), scanning electron microscopy (SEM) and FT-IR were employed to characterize the synthesized FGO/MnO2. The determination of TET at the modified electrode was studied by cyclic voltammetry (CV) and differential pulse voltammetry (DPV) in the phosphate buffer solution (PBS).TET show sharp increase in the oxidation peaks in the pH 2.Voltammetric characteristics of TET (Epa, Ipa) were estimated. From effect of scan rate, the average surface coverage (Γ) of TET on the surface of SPCE modified with FGO/MnO2 nanocomposite, the electron transfer coefficient and electron transfer constant rate ket was obtained as 10.56×1014 molecule cm-2, 0.5, and 10.41 cm.s-1respectively. Under the optimal conditions, the peak current shows linear relationship with concentration of Tetracycline (TET) ranges 1–9 μM with the detection limit of 0.2μ M. The modified SPCE was successfully used to detect TET
A rapid high performance liquid chromatography method for the determination of sphinganine (Sa) and sphingosine (So) in urine samples by employing a silica-based monolithic column is described. The samples were first extracted using ethyl acetate and derivatized using ortho-phthaldialdehyde in the presence of 2-mercaptoethanol. C20 sphinganine was used as internal standard. Under the optimized conditions, separation was achieved using a mixture of methanol:water (93:7, v/v), column temperature at 30°C, flow rate of 1 mL min−1, and an injection volume of 10 μL. Good linearity was obtained for Sa and So over the concentration range 20–500 ng mL−1(correlation coefficients ≥0.9978). The detection limits were 0.45 ng mL−1 for Sa and
... Show MoreA simple and highly sensitive cloud point extraction process was suggested for preconcentration of micrograms amount of isoxsuprine hydrochloride (ISX) in pure and pharmaceutical samples. After diazotization coupling of ISX with diazotized sulfadimidine in alkaline medium, the azo-dye product quantitatively extracted into the Triton X-114 rich phase, dissolved in ethanol and determined spectrophotometrically at 490 nm. The suggested reaction was studied with and without extraction and simple comparison between the batch and CPE methods was achieved. Analytical variables including concentrations of reagent, Triton X-114 and base, incubated temperature, and time were carefully studied. Under the selected opti
... Show MoreIn current article an easy and selective method is proposed for spectrophotometric estimation of metoclopramide (MCP) in pharmaceutical preparations using cloud point extraction (CPE) procedure. The method involved reaction between MCP with 1-Naphthol in alkali conditions using Triton X-114 to form a stable dark purple dye. The Beer’s law limit in the range 0.34-9 μg mL-1 of MCP with r =0.9959 (n=3) after optimization. The relative standard deviation (RSD) and percentage recoveries were 0.89 %, and (96.99–104.11%) respectively. As well, using surfactant cloud point extraction as a method to extract MCP was reinforced the extinction coefficient(ε) to 1.7333×105L/mol.cm in surfactant-rich phase. The small volume of organi
... Show MoreA solid Phase Extraction (SPE) followed by HPLC-UV method is described for the simultaneous quantitative determination of nine priority pollutant phenols : Phenol, 2- and 4-Nitrophenol, 2,4-Dimethylphenol, 2-, 2,4-Di-, 2,4,6-Tri-, and Penta- chlorophenol, 4 Chloro-3-methylphenol. The phenols were separated using a C-18 column with UV detector at wave length of 280nm. The Flow of mobile phase was isocratic consisted of 50:50 Acetonitrile: phosphate buffer pH=7.1, column temperature 45 C°, Flow Rate 0.7 ml/min. Calibration curves were linear (R2 = 0.9961-0.9995). The RSDs (1.301-5.805)%, LOD(39.1- 412.4) µg/L, LOQ(118.5-1250.8) µg/L, the Robustness (1.55-4.89), Ruggedness (2.82-4.00), Repeatability (2.1-4.95), Recoveries%
... Show MoreA simple and highly sensitive cloud point extraction process was suggested for preconcentration of micrograms amount of isoxsuprine hydrochloride (ISX) in pure and pharmaceutical samples. After diazotization coupling of ISX with diazotized sulfadimidine in alkaline medium, the azo-dye product quantitatively extracted into the Triton X-114 rich phase, dissolved in ethanol and determined spectrophotometrically at 490 nm. The suggested reaction was studied with and without extraction and simple comparison between the batch and CPE methods was achieved. Analytical variables including concentrations of reagent, Triton X-114 and base, incubated temperature, and time were carefully studied. Under the selected optimum conditions,
... Show MoreMetoclopramide (MCP) ion selective electrodes based on metoclopramide-phosphotungstic acid (MCP-PT) ion pair complex in PVC matrix membrane were constructed. The plasticizers used were tri-butyl phosphate (TBP), di-octyl phenyl phosphonate (DOPP), di-butyl phthalate (DBPH), di-octyl phthalate (DOP), di-butyl phosphate (DBP), bis 2-ethyl hexyl phosphate (BEHP). The sensors based on TBP, DOPP, DBPH and DOP display a fast, stable and linear response with slopes 59.9, 57.7, 57.4, 55.3 mV/decade respectively at pH ranged 2-6. The linear concentration range between 1.0×10-5 – 1.0×10-2 M with detection limit 3.0×10-6 and 4.0×10-6 M for electrodes using TBP, DOPP and DBPH while e
... Show MoreThe determination hardness in water raised to rivers caused several problem in the validity of the water used depends on where determination ions concentration calcium and magnesium in salts carbonate and sulfate , this possibility of separation between of these ions and the resulting impact on concentration and determination the degree of hardness water and appreciation between the insolvent water quality . It study the effect of the impact of concentration magnesium ion in determination the quality of the water has turned out to be Mg concentration more than 60% of the total content of hardness is borderline in hardness effect the determination. Adopted in this research determination the ions in two method titration by EDTA solution and
... Show MoreA spectrophotometric method has been proposed for the determination of two drugs containing phenol group [phenylephrine hydrochloride (PHP) and salbutamol sulphate (SLB)] in pharmaceutical dosage forms. The method is based on the diazotization reaction of metoclopramide hydrochloride (MCP) and coupling of the diazotized reagent with drugs in alkaline medium to give intense orange colored product (?max at 470 nm for each of PHP and SLB). Variable parameters such as temperature, reaction time and concentration of the reactants have been analyzed and optimized. Under the proposed optimum condition, Beer’s law was obeyed in the concentration range of 1-32 and 1-14 ?g mL-1 for PHP and SLB, respectively. The limit of detection (LOD) and l
... Show MoreTwo 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 MoreSince its first description as a cytotoxic agent, Olea europaea leaves extract gained significant popularity against human breast cancer, ethyl acetate extract of Olea europaea leaves obtained by acid hydrolysis method was evaluated in vitro as cytotoxic agent against new human breast cancer (AMJ13) cell line, using the MTT assay. One main pentacyclic triterpenoid; oleanolic acid, was isolated from leaves of Olea europaea by well-known two different methods, but not used for this compound before, the acidic hydrolysis method and basic acidic method. The presence of oleanolic acid was proved in both methods with qualitative and quantitative d
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