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 present study describes employing zero-, 1st - and 2nd -order derivative spectrophotometric methods have been developed for determination of lorazepam (LORA) and clonazepam (CLON) in commercially available tablets. LORA was determined by means of 1st (D1), 2nd (D2) derivative spectrophotometric techniques using zero cross, peak height, and Peak area. D1 used for the determination of CLON by using zero cross and peak height while D2 (zero cross) was used for the determination of CLON. The method was established to be linear in concentration containing different ratios of LORA and CLON range of (20-200 mg/L) and (5-35 mg/L) at wavelength range (250 -370 nm), (210-370nm) respectively. The proposed techniques are highly sensitive, precise a
... Show MoreThe objective of this study is to determine the concentration of copper and lead (mg/L) in drinking water by using absorption spectrophotometic and Atomic Absorption spectrophotometric method from different area in Baghdad and with different intervals , The results show that the concentration of copper and Lead ( mgL) in tap water which remains motionless in plumbing system for following periods one hours, 3 hours, 6 hours, 12 hours, 24 hours, 7 days and 14 days are (1 , 2.2 , 4 , 5.3 , 7.5 , 10 and 16 mgL copper ) & ( 0.3, 0.5 , 0.8 , 1 , 2.5 , 3 , 3.8 mg /L lead ) respectively .from these results its clear that high levels of copper & Lead occur if tap water comes in contact with copper - lead plumbing and copper lead -containing fix
... Show MoreA simple analytical method was used in the present work for the simultaneous quantification of Ciprofloxacin and Isoniazid in pharmaceutical preparations. UV-Visible spectrophotometry has been applied to quantify these compounds in pure and mixture solutions using the first-order derivative method. The method depends on the first derivative spectrophotometry using zero-cross, peak to baseline, peak to peak and peak area measurements. Good linearity was shown in the concentration range of 2 to 24 μg∙mL-1 for Ciprofloxacin and 2 to 22 μg∙mL-1 for Isoniazid in the mixture, and the correlation coefficients were 0.9990 and 0.9989 respectively using peak area mode. The limits of detection (LOD) and limits of quantification (LOQ) wer
... Show MoreObjective: The aim of this work was to detect terpenes other than boswellic acid derivatives in olibanum of Boswellia Serrata found in Iraq. Methods: The olibanum of Boswellia Serrata was macerated in methanol for one day, then filtration. Filter at was concentrated till reddish brown syrupy residue was gained, (3%) potassium hydroxide was added till basification. This basic solution was stirred continuously until a uniform emulsion was formed, then extracted with chloroform in a separatory funnel; the chloroform fraction was analyzed by GC /MS spectrometry. Results: GC /MS analysis reveal the presence of terpenes and non-terpenes constituents. Conclusion: Most of the detected terpenes were sesquiterpenes and the least one was di-terpenes.
Background: Osteoporosis is denoted by low bone mass and microarchitectural breakdown of bone tissue, directing to increased fracture risk and bone fragility. Fractures may lead to a decreased quality of life and increased medical costs. Thus, osteoporosis is widely considered a significant health concern.
Objective. This study aimed to compare quantitative computed tomography (QCT) and dual-energy X-Ray absorptiometry (DXA) to detect osteoporosis in postmenopausal women.
Subjects and Methods. We measured spinal volumetric bone mineral density (BMD) with QCT and areal spinal and hip BMD with DXA in 164 postmenopausal women. We calculated the osteo
... Show MoreThe aim of this research is to measure the effect of Adey- Shire model in the achievement and critical thinking of first intermediate female students in mathematics. The researcher adopted the experimental method with a post-test, the research of sample consists of (60) female students, divided into two groups with (30) students in the experimental group, that studied with Adey- Shire model, and (30) students in the control group who studied in the usual way. The two groups are equivalent in many variables. The researcher makes two tests of multiple choices, the first one is an achievement test consists (30) items and another test was for a critical thinking test with (25) items. The statistical analysis make to both tests is made with s
... Show MoreA 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 MoreA new method for construction ion-selective electrode (ISE) by heating reaction of methyl orange with ammonium reineckate using PVC as plasticizer for determination methyl orange and determination Amitriptyline Hydrochloried drug by formation ion-pair on electrode surface . The characteristics of the electrode and it response as following : internal solution 10-4M , pH (2.5-5) ,temperature (20-30) and response time 2 sec. Calibration response for methyl orange over the concentrationrange 10-3 -10-9 M with R=0.9989 , RSD%=0.1052, D.O.L=0.315X10-9 MEre%=(-0.877- -2.76) , Rec%.=(97.230 -101.711) .