Dapagliflozin is a novel sodium-glucose cotransporter type 2 inhibitor. This work aims to develop a new
validated sensitive RP-HPLC coupled with a mass detector method for the determination of dapagliflozin, its
alpha isomer, and starting material in the presence of dapagliflozin major degradation products and an internal
standard (empagliflozin). The separation was achieved on BDS Hypersil column (length of 250mm, internal
diameter of 4.6 mm and 5-μm particle size) at a temperature of 35℃. Water and acetonitrile were used as
mobile phase A and B by gradient mode at a flow rate of 1 mL/min. A wavelength of 224nm was selected to
perform detection using a photo diode array detector. The method met the requirement of the International
Conference on Harmonisation for Registration of Pharmaceuticals for Human Use (ICH) for validation. The
molecular weight of impurities and degradation products was estimated using positive ESI-MS. Fifteen
impurities were detected during the analysis of dapagliflozin APIs and the brand Farxiga ® and some generic
products. Three of fifteen detected impurities (H, J and K) exceeded the impurities acceptable limits 0.1%.
Those impurities were isolated using new preparative chromatography then characterized using elemental
analysis, FTIR and NMR.
In this research, annealed nanostructured ZnO catalyst water putrefaction system was built using sun light and different wavelength lasers as stimulating light sources to enhance photocatalytic degradation activity of methylene blue (MB) dye as a model based on interfacial charges transfer. The structural, crystallite size, morphological, particle size, optical properties and degradation ability of annealed nanostructured ZnO were characterized by X-Ray Diffraction (XRD), Atomic Force Microscopy (AFM) and UV-VIS Spectrometer, respectively. XRD results demonstrated a pure crystalline hexagonal wurtzite with crystalline size equal to 23 nm. From AFM results, the average particle size was 79.25nm. All MB samples and MB with annealed nanostr
... Show MoreThe main objective of this paper is to develop and validate flow injection method, a precise, accurate, simple, economic, low cost and specific turbidimetric method for the quantitative determination of mebeverine hydrochloride (MbH) in pharmaceutical preparations. A homemade NAG Dual & Solo (0-180º) analyser which contains two identical detections units (cell 1 and 2) was applied for turbidity measurements. The developed method was optimized for different chemical and physical parameters such as perception reagent concentrations, aqueous salts solutions, flow rate, the intensity of the sources light, sample volume, mixing coil and purge time. The correlation coefficients (r) of the developed method were 0.9980 and 0.9986 for
... Show MoreThe main objective of this paper is to develop and validate flow injection method, a precise, accurate, simple, economic, low cost and specific turbidimetric method for the quantitative determination of mebeverine hydrochloride (MbH) in pharmaceutical preparations. A homemade NAG Dual & Solo (0-180º) analyser which contains two identical detections units (cell 1 and 2) was applied for turbidity measurements. The developed method was optimized for different chemical and physical parameters such as perception reagent concentrations, aqueous salts solutions, flow rate, the intensity of the sources light, sample volume, mixing coil and purge time. The correlation coefficients (r) of the developed method were 0.9980 and 0.9986 for cell
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The varied applications of polystyrene in various fields of life led to examining the cause of radiation influence on some rheological behavior of commercial Polystyrene (PS) solution in the chloroform (CHCl3) solvent. Polystyrene grains shape samples were irradiated using the radioactive element Cesium- 137 with (9 µci) activity for 10, 20, and 30 minutes. The viscosity of the polymer solution depends on the concentration and size (i.e. molecular weight) of the dissolved polymer. Experimental data showed that the radiation dose affected the value of viscosity (shear, relative, specific, and reduced). The viscosity value significantly reduced at 10 min radiation dose and when increasing the dose, the viscosity value increased
... Show Moreلقد كان حرص المؤلف على إصدار هذا الكتاب نابعا ً من قناعة تامة بأن مجال التقويم والقياس بحاجة إلى كتاب علمي حديث يتناول عرض أدوات الاختبار والقياس والمتمثلة بالصدق والثبات ويتسم بالوضوح في التعبير عن المفاهيم والمصطلحات والأنواع لكل منها ليكون وسيلة مبسطة بأيدي الأساتذة والباحثين وطلبتي الدراسات العليا الماجستير والدكتوراه لإستخراج صدق وثبات الاختبارات والمقاييس بطرق إحصائية متقدمة من خلال إستخدام البرنا
... Show MoreABSTRACT 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
... Show MoreThe speaker identification is one of the fundamental problems in speech processing and voice modeling. The speaker identification applications include authentication in critical security systems and the accuracy of the selection. Large-scale voice recognition applications are a major challenge. Quick search in the speaker database requires fast, modern techniques and relies on artificial intelligence to achieve the desired results from the system. Many efforts are made to achieve this through the establishment of variable-based systems and the development of new methodologies for speaker identification. Speaker identification is the process of recognizing who is speaking using the characteristics extracted from the speech's waves like pi
... Show MoreIn this study, different methods were used for estimating location parameter and scale parameter for extreme value distribution, such as maximum likelihood estimation (MLE) , method of moment estimation (ME),and approximation estimators based on percentiles which is called white method in estimation, as the extreme value distribution is one of exponential distributions. Least squares estimation (OLS) was used, weighted least squares estimation (WLS), ridge regression estimation (Rig), and adjusted ridge regression estimation (ARig) were used. Two parameters for expected value to the percentile as estimation for distribution f
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