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bsj-7596
Qualitative and Quantitative Determination of Dapagliflozin Propanediol Monohydrate and Its Related Substances and Degradation Products Using LC-MS and Preparative Chromatography Methods
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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.

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Publication Date
Tue Dec 01 2020
Journal Name
Baghdad Science Journal
Determination of Phosphodiesterase Type 5 Enzyme (PDE-5) Inhibitors and Analogues as Adulterants in Selected Herbal Products using Gas Chromatography–Electron Impact-Mass Spectrometer (GC-EI-MS)
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       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

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Publication Date
Thu Jun 01 2023
Journal Name
Baghdad Science Journal
Determination of essential and trace elements in various vegetables using ICP-MS
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Metal 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.

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Publication Date
Sun Aug 01 2021
Journal Name
Sensors And Actuators B: Chemical
Sensitive and simple colorimetric methods for visual detection and quantitative determination of semicarbazide in flour products using colorimetric reagents
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After 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

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Publication Date
Wed Oct 28 2020
Journal Name
Iraqi Journal Of Science
A Review: Protein Identification by LC-MS: Principles, Instrumentation, and Applications: Protein Identification by LC-MS
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This 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

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Publication Date
Sat Oct 28 2023
Journal Name
Baghdad Science Journal
Indirect Flow Injection Spectrophotometric and Chromatographic Methods for the Determination of Mebendazole in Pharmaceutical Formulations
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Chromatographic 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

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Publication Date
Sun Jan 01 2017
Journal Name
Analytical Methods
Determination of pharmaceuticals in freshwater sediments using ultrasonic-assisted extraction with SPE clean-up and HPLC-DAD or LC-ESI-MS/MS detection
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A robust and sensitive analytical method is presented for the extraction and determination of six pharmaceuticals in freshwater sediments.

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Publication Date
Thu Feb 16 2023
Journal Name
Iraqi Journal Of Pharmaceutical Sciences ( P-issn 1683 - 3597 E-issn 2521 - 3512)
Qualitative and Quantitative Estimation or Chemical Constituents from Leaves and Roots of Iraqi Agave Attenuata by GC-MS and RP-HPLC(Conference Paper) #
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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

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Publication Date
Sun Jan 30 2022
Journal Name
Iraqi Journal Of Science
Determination of Active Phytochemical Compounds of Alhagi Maurorum using Gas Chromatography-Mass Spectroscopy (GC-MS)
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Alhagi 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

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Publication Date
Sun Dec 04 2011
Journal Name
Baghdad Science Journal
Quantitative and Qualitative detect for cheat beef with chicken meat by immunological methods
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beef 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

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Publication Date
Sun Jun 05 2016
Journal Name
Baghdad Science Journal
Flame Atomic Emission and Colorimetric Methods for the Determination of Cephalexin Monohydrate in Pharmaceutical Preparations
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We 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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