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.
Two simple methods spectrophotometric were suggested for the determination of Cefixime (CFX) in pure form and pharmaceutical preparation. The first method is based without cloud point (CPE) on diazotization of the Cefixime drug by sodium nitrite at 5Cº followed by coupling with ortho nitro phenol in basic medium to form orange colour. The product was stabilized and measured 400 nm. Beer’s law was obeyed in the concentration range of (10-160) μg∙mL-1 Sandell’s sensitivity was 0.0888μg∙cm-1, the detection limit was 0.07896μg∙mL-1, and the limit of Quantitation was 0.085389μg∙mL-1.The second method was cloud point extraction (CPE) with using Trtion X-114 as surfactant. Beer
... 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 MoreThis paper presents a grey model GM(1,1) of the first rank and a variable one and is the basis of the grey system theory , This research dealt properties of grey model and a set of methods to estimate parameters of the grey model GM(1,1) is the least square Method (LS) , weighted least square method (WLS), total least square method (TLS) and gradient descent method (DS). These methods were compared based on two types of standards: Mean square error (MSE), mean absolute percentage error (MAPE), and after comparison using simulation the best method was applied to real data represented by the rate of consumption of the two types of oils a Heavy fuel (HFO) and diesel fuel (D.O) and has been applied several tests to
... Show MoreThe current study performed in order to detect and quantify epicatechin in two tea samples of Camellia sinensis (black and green tea) by thin layer chromatography (TLC) and high performance liquid chromatography (HPLC). Extraction of epicatechin from black and green tea was done by using two different methods: maceration (cold extraction method) and decoction (hot extraction method). Qualitative and quantitative determinations of epicatechin in two tea samples were investigated. Epicatechin identification was made by utilizing preliminary chemical tests and TLC. This identification was also boosted by HPLC and then quantified epicatechin in all ethyl acetate fractions of two tea samples. This research revealed the existence of epica
... Show MoreTwo simple and sensitive spectrophotometric methods are proposed for the determination of amitriptyline in its pure form and in tablets. The first method is based on the formation of charge- transfer complex between amitriptyline as n-donor and tetracyano-ethylene (TCNE) as πacceptor. The product exhibit absorbance maximum at 470 nm in acetonitrile solvent (pH =9.0 ) . In the second method the absorbance of the ion- pair complex, which is formed between the soughted drug and bromocresol green (BCG), was measured at 415 nm at ( pH=3.5) . In addition to classical univariate optimization, modified simplex method (MSM) was applied in the optimization of the variable affecting the color producing reaction by a geometric simple
... Show MoreOne of the serious problems in any wireless communication system using multi carrier modulation technique like Orthogonal Frequency Division Multiplexing (OFDM) is its Peak to Average Power Ratio (PAPR).It limits the transmission power due to the limitation of dynamic range of Analog to Digital Converter and Digital to Analog Converter (ADC/DAC) and power amplifiers at the transmitter, which in turn sets the limit over maximum achievable rate.
This issue is especially important for mobile terminals to sustain longer battery life time. Therefore reducing PAPR can be regarded as an important issue to realize efficient and affordable mobile communication services.
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Background: Despite the importance of vaccines in preventing COVID-19, the willingness to receive COVID-19 vaccines is lower among RA patients than in the general population. Objective: To determine the extent of COVID-19 knowledge among RA patients and their attitudes and perceptions of COVID-19 vaccines. Methods: A qualitative study with a phenomenology approach was performed through face-to-face, individual-based, semi-structured interviews in the Baghdad Teaching Hospital, Baghdad, Iraq, rheumatology unit. A convenient sample of RA patients using disease-modifying anti-rheumatic drugs was included until the point of saturation. A thematic content analysis approach was used to analyze the obtained data. Results: Twenty-five RA pa
... Show MoreThe aim of this study is to screen the phytochemicals found in Populus euphratica leaves since this type of trees are used traditionally by many villagers as treatment for eczema and other skin disease and also this plant is poorly investigated for their phytochemicals especially in Iraq. Phytochemical screening of the extracts obtained from the n-hexane and chloroform fraction of leaves of Populus euphratica was done by Thin-layer chromatography and various spraying reagents to test if alkaloids, sterols and other compounds are present. UPLC-electrospray ionization –tandem mass spectroscopy along with GC-MS and HPTLC are used to identify the phytochemicals present in the plant leaves.UPLC-ESI-MS/MS method 20 compound
... Show MoreIn this study, simple, low cost, precise and speed spectrophotometric methods development for evaluation of sulfacetamide sodium are described. The primary approach contains conversion of sulfacetamide sodium to diazonium salt followed by a reaction with p-cresol as a reagent in the alkaline media. The colored product has an orange colour with absorbance at λmax 450 nm. At the concentration range of (5.0-100 µg.mL-1), the Beer̆ s Low is obeyed with correlation coefficient (R2= 0.9996), limit of detection as 0.2142 µg.mL-1, limit of quantification as 0.707 µg.mL-1 and molar absorptivity as 1488.249 L.mol-1.cm-1. The other approach, cloud point extraction w
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