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 paper we proposed the method of X-ray fluorescence (XRF) determination of some essential trace elements in medicinal herbs and vitamin-mineral complexes at the level of 100-101 mg/ml. To increase sensitivity and selectivity of the determination we simple and effective approach based on the extraction of metal ions from aqueous solutions with chemically modified polyurethane foam sorbents followed by direct XRF analysis. The conditions of sorption preconcentration of Co(II), Ni(II) and Zn(II) ions with modified sorbents were optimized. The proposed approach is used for the determination of trace elements in several kinds of medicinal herbs (coltsfoot leaves, nettle leaves and yarrow herb) and vitamin-mineral
... Show MoreBackground: This study was conducted to evaluate the hard palate bone density and thickness during 3rd and 4th decades and their relationships with body mass index (BMI) and compositions, to allow more accurate mini-implant placement. Materials and method: Computed tomographic (CT) images were obtained for 60 patients (30 males and 30 females) with age range 20-39 years. The hard palate bone density and thickness were measured at 20 sites at the intersection of five anterioposterior and four mediolateral reference lines with 6 and 3 mm intervals from incisive foramen and mid-palatal suture respectively. Diagnostic scale operates according to the bioelectric impedance analysis principle was used to measure body weight; percentages of body fa
... 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 study, advanced oxidation treatment, the TiO2 /UV/H2O2 process was applied to decolorisation of the reactive yellow dyes in aqueous solution. The UV radiation was carried out with a 6 W low-pressure mercury lamp. The rate of color removal was studied by measuring the absorbency at a characteristic wavelength. The effects of H2O2 dosage, dye initial concentration and pH on decolorisation kinetics in the batch photoreactor were investigated. The highest decolorisation rates were observed (98.8) at pH range between 3 and 7. The optimal levels of H2O2 needed for the process were examined. It appears that high levels of H2O2 could reduce decolori
... Show MoreA new Spectrophotometric method, is for individual and simultaneous determination of Ciprofloxacin hydrochloride(CIP) and Mebeverin hydrochloride(MEB) by the first and second derivative mode techniques. The first and second derivative spectra of these compounds permitted individual and simultaneous determination of CIP and MEB in concentration range of (4-28μg/mL) by measuring the amplitude of peak- to- base line and the area under peak at selected spectrum intervals. The methods showed a reasonable precision and accuracy and have been applied to determine CIP and MEB in four different pharmaceutical preparations.
A simple, sensitive and accurate spectrophotometric method has been developed for the determination of salbutamol sulphate (SAB) and isoxsuprine hydrochloride (ISX) in pure and pharmaceutical dosage. The method involved oxidation of (SAB) and (ISX) with a known excess of N-bromosuccinamid in acidic medium, and subsequent occupation of unreacted oxidant in decolorization of Evans blue dye (EB). This, in the presence of SAB or ISX was rectilinear over the ranges 1.0-12.0, 1.0-11.0 µg/mL, with molar absorptivity 4.21×104 and 2.58×104 l.mol-1.cm-1 respectively. The developed method had been successfully applied for the determination of the studied drugs in their pharmaceutical dosage resulting i
... Show MoreTo determine the relationship between celiac disease and reproductive disorder, twenty two women with recurrent spontaneous abortion (18-35) years have been investigated from the period 2017/11/1 – 2018/2/1 and compared wih twenty two parentally healthy women. All studied groups were carried out to measure antitissue transglutaminase IgA and IgG antibodies by Enzyme linked immunosorbent assay (ELISA) technique, There were a highly significant differences (P < 0.01) in the concentration of anti TtG IgA and IgG Ab compared to control group, while there was non-significant differences (P > 0.05) in the concentration of anti TtG IgA according to the age group and there was a significant difference (P < 0.05) in the concentration of anti TtG I
... Show MoreCefixime (CFX) was treated with sodium nitrite and hydrochloric acid for diazotization reaction followed by coupling with ?-Naphthol in alkaline medium to form, a yellow colored azo dye compound which exhibits maximum absorption (?max) at 412 nm where the concentration of (CFX) was determined spectrophotometrically. The optimum reaction conditions and other analytical parameters were evaluated. Beer’s law was obeyed in the concentration range of (1-20) ?g.mL-1 with a molar absorptivity of 34870.5 L.mol-1.cm-1. The limit of detection was found to be 0.1090 ?g.mL-1 and the Sandell's sensitivity value was 0.0130 ?g.cm-2. The proposed method could be successfully applied to
... Show MoreNicotine was separated from eggplant and green pepper seeds (Solanaceous) by High Performance Liquid Chromatography (HPLC).The concentration of nicotine in the eggplant extract (0.871-0.877 μg/ml) was determined by injecting standard material with 0.5 and 1.5 μg/ml, while the concentrations of nicotine in green pepper extract (0.613-0.618 μg/ml) was determined when the standard material was injected with 0.5 and 1.5 μg/ml. The qualitative chemical data was calculated from derivations of the standard material. Nicotine concentration was measured qualitatively in both extracts through the calibration curve and method of the standard addition. This technique has high accuracy and compatibility, bringing the proportion of relati
... Show MoreBackground: The beliefs of pharmacy students in their curriculum may be critical to the success of medical education and the development of global health competences. Objective: To assess the beliefs, attitudes, and obstacles of PharmD students at the College of Pharmacy, University of Baghdad, during their first year in the newly adopted PharmD program. Method: In-depth qualitative interviews were conducted using flexible probing approaches. A sample of fourth-year PharmD students from the University of Baghdad's College of Pharmacy was selected using a purposive sampling method. The gathered data was analyzed using a thematic content analysis approach. Results: 40% of participants applied for the program because they believed it w
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