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.
The 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 MoreAbstract
This work is considered the first study for the components of the Iraqi Leucaena leucocephala plant, where the different phytochemical compounds that present in the aerial parts were identified by using the gas chromatography/mass spectrometry technique (GC/MS). The type of the components and their concentration will differ according to the part of the plant used and the method of extraction (hot and cold). This study made a comparison in lupeol concentration that was identified and isolated from petroleum ether fractions of Leucaena leucocephala by using Gas Chromatography/Mass Spectrometry (GC/MS), High-performance thin-layer chromatography (HPTLC), and Preparative High-Performance Li
... 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
... Show MoreKetoprofen has recently been proven to offer therapeutic potential in preventing cancers such as colorectal and lung tumors, as well as in treating neurological illnesses. The goal of this review is to show the methods that have been used for determining ketoprofen in pharmaceutical formulations. Precision product quality control is crucial to confirm the composition of the drugs in pharmaceutical use. Several analytical techniques, including chromatographic and spectroscopic methods, have been used for determining ketoprofen in different sample forms such as a tablet, capsule, ampoule, gel, and human plasma. The limit of detection of ketoprofen was 0.1 ng/ ml using liquid chromatography with tandem mass spectrometry, while it was 0
... Show MoreFlow-injection (FI) spectrophotometric method has been developed for the analysis of thymol in pharmaceutical preparations. The method is based on organic coupling reaction between thymol and 4-amino antipyrine in the presence of alkaline medium to form an intense stable red color complex with copper nitrate that has a maximum absorption at 490 nm. Optimum conditions for determination of the drug was investigated .The calibration graph was linear over the range of 5-500 µg.ml-1 of thymol . The limit of detection (LOD) and limit of quantification (LOQ) were 1.81 ?g mL-1 and 3.60 ?g mL-1 respectively .The proposed method was applied satisfactorily to the determination of thymol in mouth wash preparations. The procedure is characterized by
... Show MoreThis approach was developed to achieve an accurate, fast, economic and sensitivity to estimation of diphenhydramine Hydrochloride. The dye that produced via reaction between diphenhydramine HCl with thymol blue in acidic medium pH ≈ 4.0. The ion pair method include an optimization study to formed yellowcolored that extraction by liquid – liquid method. The product separated of complexes by using by chloroform solution measured spectrophotometry at 400 nm. The analysis data at optimum conditions showed that linearity concentration in a range of calibration curve 1.0 – 50 μg /mL, limit of detectionand limit of quantification 0.0786 and 0.2358 μg/mL respectively. The molar absorptivity and Sandell’s sensitivity were 1.8 × 10 -4 L/mo
... Show MoreA rapid, sensitive and without extraction spectrophotometric method for determination of clonazepam (CLO) in pure and pharmaceutical dosage forms has been described. The proposed method was simply depended on charge transfer reaction between reduced CLO (n-donor) and metol (N-methyl-p-aminophenol sulfate) as a chromogenic reagent (π- acceptor). The reduced drug, with zinc and concentrated hydrochloric acid, produced a purple colored soluble charge-transfer complex with metol in the presence of sodium metaperiodate in neutral medium, which has been measured at λmax 532 nm. All the variables which affected the developed and the stability of the colored product such as concentration of reagent and oxidant, temperature and time of rea
... Show MoreTwo field experiments were carried out for cultivating yellow maize crop Zea mays L. during the autumn planting season 2019 in two sites with soils of different textures. The first site is a loamy texture in one of the fields of the Medhatia Agriculture Division, Babylon Governorate. The second was silty loam by an alluvial mixture in one of the fields of Al-Nouriah Research Station, Ministry of Agriculture located in Al-Nouriah sub-district, Al-Qadisiyah governorate. It was found through the results that the uniformity, efficiency, and adequacy of the irrigation efficiency of the sprinkler irrigation method is better than that of the sprinkler irrigation method, and it ranged between (88.6-88.7) for uniformity and (84-86)% of the irrigatio
... Show More