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.
Sildenafil, tadalafil, and vardenafil are phosphodiesterase type 5 enzyme (PDE-5) inhibitors used for the treatment of male erectile dysfunction. This present study aims to investigate 55 herbal products indicated for men’s sexual health from the Malaysian market for adulteration of PDE-5 inhibitors and analogues. The screening and identification of 20 PDE-5 inhibitors and analogues in herbal products of various forms (powder, capsules, tablets, and pastels) were conducted using gas chromatography–electron impact-mass spectrometer (GC-EI-MS). The analysis has shown that 19 herbal products were adulterated with PDE-5 inhibitors and analogues. Unique ion fragmentations and the presence of molecular
... Show MoreMetal contents in vegetables are interesting because of issues related to food safety and potential health risks. The availability of these metals in the human body may perform many biochemical functions and some of them linked with various diseases at high levels. The current study aimed to evaluate the concentration of various metals in common local consumed vegetables using ICP-MS. The concentrations of metals in vegetables of tarragon, Bay laurel, dill, Syrian mesquite, vine leaves, thymes, arugula, basil, common purslane and parsley of this study were found to be in the range of, 76-778 for Al, 10-333 for B, 4-119 for Ba, 2812-24645 for Ca, 0.1-0.32 for Co, 201-464 for Fe, 3661-46400 for K, 0.31–1.
... Show MoreAfter baking the flour, azodicarbonamide, an approved food additive, can be converted into carcinogenic semicarbazide hydrochloride (SEM) and biurea in flour products. Thus, determine SEM in commercial bread products is become mandatory and need to be performed. Therefore, two accurate, precision, simple and economics colorimetric methods have been developed for the visual detection and quantitative determination of SEM in commercial flour products. The 1st method is based on the formation of a blue-coloured product with λmax at 690 nm as a result of a reaction between the SEM and potassium ferrocyanide in an acidic medium (pH 6.0). In the 2nd method, a brownish-green colored product is formed due to the reaction between the SEM and phosph
... Show MoreThis review will focus on protein and peptide separation studies of the period 1995 to 2010. Peptide and protein analysis have developed dramatically after applying mass spectrometry (MS) technology and other related techniques, such as two-dimensional liquid chromatography and two-dimensional gel electrophoresis. Mass spectrometry involves measurements of mass-to-charge ratios of the ionized sample. High-performance liquid chromatography (HPLC) is an important technique that is usually applied before MS is conducted due to its efficient separation. Characterization of proteins provides a foundation for the fundamental understanding of biology aspects. In this review, instrumentation, principle, applications, developments, and accuracy o
... Show MoreChromatographic and spectrophotometric methods for the estimation of mebendazole in
pharmaceutical products were developed. The flow injection method was based on the oxidation of
mebendazole by a known excess of sodium hypochlorite at pH=9.5. The excess sodium hypochlorite is then
reacted with chloranilic acid (CAA) to bleach out its color. The absorbance of the excess CAA was recorded
at 530 nm. The method is fast, simple, selective, and sensitive. The chromatographic method was carried out
on a Varian C18 column. The mobile phase was a mixture of acetonitrile (ACN), methanol (MeOH), water
and triethylamine (TEA), (56% ACN, 20% MeOH, 23.5% H2O, 0.5% TEA, v/v), adjusted to pH = 3.0 with
1.0 M hy
A robust and sensitive analytical method is presented for the extraction and determination of six pharmaceuticals in freshwater sediments.
This research concentrate on cultivated Iraqi Agave attenuata dried leaves and roots, because of little studies on this plant especially on the root that lead to the eager of study and comparison of phytochemical constituents between leaves and root. Extraction of bioactive constituents was carried out using several solvents with increasing polarity (n-hexane, ethyl acetate and methanol) by soxhlet apparatus. Steroidal saponins in Agave genus is well documented in many species, lightening the minds in this research on extraction method which is specific for steroidal saponins. Phytochemical screening was done by GC/MS for n-hexane fraction, qualitative and quantitative estimation of several bioactive constituents (caffe
... Show MoreAlhagi maurorum (camel thorn) is a grayish, evergreen, deeply rooting plant that has spiny needle -like branches. In our study, the phytochemical contents of the root ethanoloic extract of A. maurorum were determined by using gas chromatography-mass spectroscopy (GC-MS). Thirty two chemical constituents were identified. We revealed the existence of oxalic acid, anti-2 acetoxyacetaldoxime, sulfone, butyl isopropyl, 2,3-pentanedione, 2-butanone, n,n,o triacetylhydroxylamine. di(1,2,5-oxadiazole)[3,4-b;3,4-e]pyrazine, isobutane,3,4-hexanedione,3-hexanone, pentane, 3-pentanone, 3-butene, 2-thiopheneacetic acid, 2-pyrazoline, 4-hepten-3-onemethylphosphonic acid, butane, propanoic acid, methane, azetidine, heptane, butanoic a
... Show Morebeef and chicken meat were used to get Sarcoplasim, the chicken Sarcoplasim were used to prepare antibody for it after injected in rabbit, the antiserums activity were 1/32 by determined with Immune double diffusion test, the self test refer to abele for some antiserums to detected with beef sarcoplasim, which it mean found same proteins be between beef and chicken meat, which it refer to difficult depended on this immune method to detect for cheat of chicken meat with beef, so the antibody for beef sarcoplasim were removed from serum by immune absorption step to produce specific serum against chicken sarcoplasim that it used in Immune double diffusion test to qualitative detect for cheat beef with 5% chicken meat or more at least, and the
... Show MoreWe propose two simple, rapid, and convenient spectrophotometric methods which are described for the determination of cephalexin in bulk and its pharmaceutical preparations. They are based on the measurement of the flame atomic emission of potassium ion (in the first method) and colorimetric determination of the green colored solution at 610 nm formed after the reaction of cephalexin with potassium permanganate as an oxidant agent (in the second method) in basic medium. The working conditions of the methods are investigated and optimized. Beer's law plot shows a good correlation in the concentration range of 5-40?g ml-1. The detection limits are 2.573,2.814 ?g ml-1 for the flame emission photometric method and 1.844,2.016 ?g ml-1 for colo
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