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.
A method was developed that offers a rapid, simple and accurate technique for the determination of chlorophenols at trace levels in aqueous samples with very limited volumes of organic solvents. These compounds were acetylated, then preliminarily extracted with n-hexane. The enriched chlorophenols were directly analyzed using gas chromatography with an electron-capture detector. The detection limits were in the range of 0.001–0.005 mg/L, except for 2-chlorophenol, which was always above 0.013 mg/L. Relative standard deviation for the spiked water samples ranged from 2.2 to 6.1%, while relative recoveries were in the range of 67.1 to 101.3%.
It has been shown in ionospheric research that calculation of the total electron content (TEC) is an important factor in global navigation system. In this study, TEC calculation was performed over Baghdad city, Iraq, using a combination of two numerical methods called composite Simpson and composite Trapezoidal methods. TEC was calculated using the line integral of the electron density derived from the International reference ionosphere IRI2012 and NeQuick2 models from 70 to 2000 km above the earth surface. The hour of the day and the day number of the year, R12, were chosen as inputs for the calculation techniques to take into account latitudinal, diurnal and seasonal variation of TEC. The results of latitudinal variation of TE
... Show MoreA single step extraction-cleanup procedure using porous membrane-protected micro-solid phase extraction (μ-SPE) in conjunction with liquid chromatography–tandem mass spectrometry for the extraction and determination of aflatoxins (AFs) B1, B2, G1 and G2 from food was successfully developed. After the extraction, AFs were desorbed from the μ-SPE device by ultrasonication using acetonitrile. The optimum extraction conditions were: sorbent material, C8; sorbent mass, 20 mg; extraction time, 90 min; stirring speed, 1000 rpm; sample volume, 10 mL; desorption solvent, acetonitrile; solvent volume, 350 μL and ultrasonication period, 25 min without salt addition. Under the optimum conditions, enrichment factor of 11, 9, 9 and 10 for AFG2, AFG1
... Show MoreA modern, rapid RP-HPLC-UV method was developed and validated in compliance with FDA and EMA guidelines for simultaneous quantification of 15 βlactam antibiotics) Ampicillin, Amoxicillin, cephalexin, cefotaxime, cefoxitin, cefamandole, cephalothin, piperacillin, penicillin, oxacillin, cloxacillin, nafcillin Carbenicillin, Mezlocillin and Dicloxacillin) in pharmaceutical formulations and pure forms. The method employs Column NEUCLEODUR C-18 (4.0 mm x 100 mm, 5µm particle size), at a temperature of thirty degrees Celsius, and the mobile phase was acetonitrile and KH2PO4 using gradient elution with a total separation time of 13 minutes, a flow rate of 1.3 ml/min, at = pH 4.5 for the buffer solution and the λ max was 220 nm. The met
... Show MoreTo identify and explore the factors nurses perceive as influencing their knowledge acquisition in relation to diabetes care and its management in Saudi Arabia.
Diabetes continues to pose major healthcare challenges despite advances in diabetes management. Nurses have a crucial role in diabetes care, but diabetes knowledge deficits deter effective collaboration with other healthcare providers in educating patients about diabetes self‐management.
An exploratory descriptive qualitative design.
This research discusses the subject of emotional stimulation factors through the stages of product design interaction with the consumer and what they reflect in the formation of a self-consideration of the design in his emotional memory regarding the specific brand through the following question (What is the emotional stimulus in the design of certain products and its reflection on the consumer during the processes of receiving and using it?), The importance of the research comes in the connection of design elements with many sensory factors used and motivating to attract the consumer to the acquisition of a specific design and the demand for its experience, the study aims Detection and access to emotional stimulation in the design of th
... Show MorePesticides serve a crucial function in contemporary farming practices, safeguarding agricultural crops against pest infestations and boosting production outputs. However, indiscriminate use has caused environmental and human health damage. This study aimed to develop and validate a gas chromatography-flame ionization detection (GC-FID) methodology for the direct and routine analysis of spiromesifen residues in soil, leaves, and tomato fruits. The proposed method prioritizes simplicity by avoiding derivatization steps, offering advantages over existing approaches that utilize lengthy multi-step extraction or derivatization prior to GC analysis. A key novelty of this work is the development of a QuEChERS extraction coupled directly to GC-FID
... Show MoreAs a result of the developments that occurred in technological and digital technologies, which had a fundamental role in changing the paths of science, including the sciences of communication and the art of design, especially since these developments were the result of the information revolution, which called for the need to find alternatives that contribute to organizing presentations of information and texts in accordance with the manufacture of constructive content to deliver A communication message for the recipient to achieve culture and communication together, as it has become necessary to employ technical and digital developments in organizing that information according to the rules and laws of design and producing newspapers asso
... Show MoreThis study was aimed to develop an optimized Dy determination method using differential pulse voltammetry (DPV). The Plackett-Burman (PB) experimental design was used to select significant factors that affect the electrical current response, which were further optimized using the response surface method-central composite design (RSM-CCD). The type of electrolyte solution and amplitude modulation were found as two most significant factors, among the nine factors tested, which enhance the current response based on PB design. Further optimization using RSM-CCD shows that the optimum values for the tw
... Show MoreHigh-performance liquid chromatographic methods are used for the determination of water-soluble vitamins with UV-Vis. Detector. A reversed-phase high-performance liquid chromatographic has been developed for determination of water-soluble vitamins. Identification of compounds was achieved by comparing their retention times and UV spectra with those of standards solution. Separation was performed on a C18 column, using an isocratic 30% (v/v) acetonitril in dionozed water as mobile phase at pH 3.5 and flow rate 1.0m/min. The method provides low detection and quantification limits, good linearity in a large concentration interval and good precision. The detection limits ranged from 0.01 to 0.025µg/ml. The accuracy of the method was
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