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.
Several attempts have been made to modify the quasi-Newton condition in order to obtain rapid convergence with complete properties (symmetric and positive definite) of the inverse of Hessian matrix (second derivative of the objective function). There are many unconstrained optimization methods that do not generate positive definiteness of the inverse of Hessian matrix. One of those methods is the symmetric rank 1( H-version) update (SR1 update), where this update satisfies the quasi-Newton condition and the symmetric property of inverse of Hessian matrix, but does not preserve the positive definite property of the inverse of Hessian matrix where the initial inverse of Hessian matrix is positive definiteness. The positive definite prope
... Show MoreBored piles settlement behavior under vertical loaded is the main factor that affects the design requirements of single or group of piles in soft soils. The estimation of bored pile settlement is a complicated problem because it depends upon many factors which may include ground conditions, validation of bored pile design method through testing and validation of theoretical or numerical prediction of the settlement value. In this study, a prototype single and bored pile group model of arrangement (1*1, 1*2 and 2*2) for total length to diameter ratios (L/D) is 13.33 and clear spacing three times of diameter, subjected to vertical axial loads. The bored piles model used for the test was 2000
... Show MoreThe study aims to investigate the effect of Al2O3 and Al additions to Nickel-base superalloys as a coating layer on oxidation resistance, and structural behavior of nickel superalloys such as IN 738 LC. Nickel-base superalloys are popular as base materials for hot components in industrial gas turbines such as blades due to their superior mechanical performance and high-temperature oxidation resistance, but the combustion gases' existence generates hot oxidation at high temperatures for long durations of time, resulting in corrosion of turbine blades which lead to massive economic losses. Turbine blades used in Iraqi electrical gas power stations require costly maintenance using traditional processes regularly. These blades are made
... Show MoreBiodiesel production from microalgae depends on the biomass and lipid production. Both biomass and lipid accumulation is controlled by several factors. The effect of various culture media (BG11, BBM, and Urea), nutrients stress [nitrogen (N), phosphorous (P), magnesium (Mg) and carbonate (CO3)] and gamma (γ) radiation on the growth and lipid accumulation of Dictyochloropsis splendida were investigated. The highest biomass and lipid yield of D. splendida were achieved on BG11 medium. Cultivation of D. splendida in a medium containing 3000 mg L−1 N, or 160 mg L−1 P, or 113 mg L−1 Mg, or 20 mg L-1 CO3, led to enhanced growth rate. While u
... Show MoreIn the present investigation, bed porosity and solid holdup in viscous three-phase inverse fluidized bed (TPIFB) are determined for aqueous solutions of carboxy methyl cellulose (CMC) system using polyethylene and polypropylene as a particles with low-density and diameter (5 mm) in a (9.2 cm) inner diameter with height (200 cm) of vertical perspex column. The effectiveness of gas velocity Ug , liquid velocity UL, liquid viscosity μL, and particle density ρs on bed porosity BP and solid holdups εg were determined. The bed porosity increases with "increasing gas velocity", "liquid velocity", and "liquid viscosity". Solid holdup decreases with increasing gas, liquid
... Show MoreThe research involved a rapid, automated and highly accurate developed CFIA/MZ technique for estimation of phenylephrine hydrochloride (PHE) in pure, dosage forms and biological sample. This method is based on oxidative coupling reaction of 2,4-dinitrophenylhydrazine (DNPH) with PHE in existence of sodium periodate as oxidizing agent in alkaline medium to form a red colored product at ʎmax )520 nm (. A flow rate of 4.3 mL.min-1 using distilled water as a carrier, the method of FIA proved to be as a sensitive and economic analytical tool for estimation of PHE.
Within the concentration range of 5-300 μg.mL-1, a calibration curve was rectilinear, where the detection limit was 3.252 μg.mL
A simple, accurate, and cost-efficient UV-Visible spectrophotometric method has been developed for the determination of naphazoline nitrate (NPZ) in pure and pharmaceutical formulations. The suggested method was based on the nucleophilic substitution reaction of NPZ with 1,2-naphthoquinone-4-sulfonate sodium salt in alkaline medium at 80°C to form an orange/red-colored product of maximum absorption (λmax) at 483 nm. The stoichiometry of the reaction was determined via Job's method and limiting logarithmic method, and the mechanism of the reaction was postulated. Under the optimal conditions of the reaction, Beerʼs law was obeyed within the concentration range 0.5–50 μg/mL, the molar absorptivity value (ε) was 5766.5 L × mol–1 × c
... Show MoreGraphene oxide GO was functionalized with 4-amino, 3-substituted 1H, 1, 2, 4 Triazole 5(4H) thion (ASTT) to obtain GOT. GOT characterized by FT-IR, XRD.via modification of the working electrode of the SPCE with the prepared nanomaterial (GOT) the effect of scan rate and pH on the determination of Amoxilline (AMOX) was studied using cyclic voltammetry. AMOX show various responses at pH ranging from 2 to 7 and also was observed sharp increase in the oxidation peaks in the pH 3. The formal potential (midpoint) for AMOX was highly pH-dependent. From the effect of scan rate, surface coverage concentration Γ of electroactive species the values of the electron transfer coefficient and the electron transfer constant rate ket was obtained as 5.39×
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