Four different spectrophotometric methods are used in this study for the determination of Sulfamethoxazole and sulfanilamide drugs in pharmaceutical compounds, synthetic samples, and in their pure forms. The work comprises four chapters which are shown in the following: Chapter One: Includes a brief for Ultraviolet-Visible (UV-VIS) Absorption spectroscopy, antibacterial drugs and sulfonamides with some methods for their determination. The chapter lists two methods for optimization; univariate method and multivariate method. The later includes different types, two of these were mentioned; simplex method and design of experiment method. Chapter Two: Includes reaction of the two studied drugs with sodium nitrite and hydrochloric acid for diazotization reaction followed by coupling with diphenylamine in acidic medium to form, a blue colored azo dye compound which exhibits maximum absorption (λmax) at 530 nm for sulfamethoxazole complex and 531 nm for sulfanilamide complex against the reagent blank and the concentration of these drugs were determined spectrophotometrically. The optimum reaction conditions and other analytical parameters were evaluated. In addition to classical univariate optimization, modified simplex method has been applied in optimization of the variables affecting the color producing reaction. The results show better optical characteristics for calibration curves and statistical data were obtained under optimum conditions obtained by multi simplex optimization, in comparison with those obtained via univariate method for two studied drugs. Beer’s law obeyed in the concentration range of 0.5-12.0 μg.mL-1, 0.5-7.0 μg.mL-1 for sulfamethoxazole and sulfanilamide respectively with molar absorptivity of 4.9617×104 L.mol-1.cm-1 for sulfamethoxazole and 5.9185×104 L.mol-1.cm-1 for sulfanilamide. The detection limits were 0.036 μg.mL-1 and 0.016 µg.mL-1 for the two complexes respectively by simplex method. No interferences from the studied excipients on the determination of these drugs were found therefore, the proposed methods were applied successfully II for the determination of the sulfamethoxazole and sulfanilamide in pharmaceutical compound and in synthetic samples. Chapter Three: Is based on the formation of condensation complexes of each drug with sodium 1,2-naphthoquinon-4-sulfonate as a chromogenic reagent. The absorbance values, for the formed complexes were measured at 460 nm for sulfamethoxazole and 455 nm for sulfanilamide; against reagent blank. Different variables affecting the completion of reaction have been carefully optimized following the classical univariate sequence and design of experiment (DOE) method and the results were obtained under optimum conditions by (DOE) optimization which shows better optical characteristics for calibration curves and statistical data in comparison with those obtained via univariate method for two studied drugs. The calibration graphs are linear in the ranges of (5.0-50.0) µg.mL-1 for sulfamethoxazole and (5.0-30.0) µg.mL-1 for sulfanilamide with detection limit 0.359 µg.mL-1for sulfamethoxazole complex and 0.536 µg.mL-1 for sulfanilamide complex. The molar absorptivity was found to be (7.0918×104 L.mol-1.cm-1) for sulfamethoxazole and (7.0774×104 L.mol-1.cm-1) for sulfanilamide by the design of experiment (DOE) method. Finally no interferences from the studied excipients on the determination of these drugs were found. The proposed methods have been successfully applied for the determination of sulfamethoxazole and sulfanilamide in their pharmaceutical preparation and synthetic samples. Chapter Four: Includes two parts; Derivative spectrophotometry and partial least-squares (PLS). Derivative spectrophotometry is based on the first and second derivative spectra of absorption which has been applied for simultaneous spectrophotometric determination of sulfamethoxazole and sulfanilamide in their mixture in the ultraviolet region. The method offers an advantage of getting rid of the resulting error in the values of absorption because of the presence of each drug with the presence of interferences from the excipients. It was found that the method is able to accurately estimate sulfamethoxazole in the range of (2.0-50.0) μg.mL-1; in mixtures containing III (2.0-30.0) μg.mL-1 of sulfanilamide, as (interferent). The results obtained, with the first derivative measurements, indicate that when the concentration of sulfanilamide is kept constant and the concentration of sulfamethoxazole varied, the peak amplitudes are measured at peak-to-baseline (223, 254,287 nm), peak to peak height between (223- 254 nm), (254-287nm). Moreover, the height at the zero cross of sulfanilamide at (235.62, 258.72 nm), heightto-height of the two zero crosses between (235.62-258.72 nm) and area under peak between (241.95-267.04 nm), (267.04-330 nm) were found to be in proportion to the sulfamethoxazole concentration therefore they are used for the determination of it. The careful inspection of the second derivative spectra obtained for the mentioned mixtures of sulfamethoxazole and sulfanilamide shows that peak to basline is at (239.5, 263.5, 267.75, 301, 215 nm) , height to basline is at zero cross is at (245.86, 271.28 nm) , peak to peak is between (239.5-264.25 nm), (239.5-267.75 nm), (271.28-301 nm), (215-239.5 nm), height to height is at two zero cross (245.86-271.28 nm) in addition to peak area at the interval between (254.12-281 nm), (286.95- 329.5 nm), (221.75-254.12 nm) measurements at specified wavelength could be used to quantify the exact concentration of sulfamethoxazole in presence of sulfanilamide. Sulfanilamide was determined for the range of (2.0-50.0) μg.mL-1; in a mixture containing (2.0-50.0) μg.mL-1 of sulfamethoxazole as (interferent). The procedure gave good results over the studied range of concentration depending on peak-to-baseline at (224, 246, 271 nm), height at zero cross at (241.95, 267.04 nm), peak to peak between (224-246 nm), (246-271 nm), height to height at two zero cross (241.95-271 nm) and area under the peak at (235.62-258.72 nm) measurements were found to be used for the determination of sulfanilamide in the first derivative technique. On other situation, the wavelengths are at 218 nm, 231 nm, 260 nm and 278 nm (peak to base line measurements), and height at two zero cross at 254 nm and 281 nm, and peak to peak measurements between (218-231 nm), (231-260 nm) and (260-278 nm), and height at zero cross at (254, 281 nm), wavelengths at (210-224 nm) , (224-245.84 nm) and (271.28-330 nm) peak area at the interval measurements were used for the estimation of sulfanilamide on second derivative.
In medical practice, nonsteroidal anti-inflammatory drugs (NSAIDs) are often used to treat osteoarthritis and rheumatoid arthritis. Ibuprofen is a well-known NSAID, analgesic, and antipyretic medication. This chemical is an active ingredient of several oral medications that are offered in tablet, gel pellet, and syrup forms and has higher efficacy, tolerance, and side effect rates than other compounds, including pyrazolone derivatives. We present a unique plasma-assisted desorption/ionization mass spectrometry (PADI-MS) approach for improving pharmaceutically important solids using an ibuprofen tablet as a model solid sample. The goal of the study is to create an innovative mass spectrometric method that could be used for quick and accur
... Show MoreThis paper proposed a new method to study functional non-parametric regression data analysis with conditional expectation in the case that the covariates are functional and the Principal Component Analysis was utilized to de-correlate the multivariate response variables. It utilized the formula of the Nadaraya Watson estimator (K-Nearest Neighbour (KNN)) for prediction with different types of the semi-metrics, (which are based on Second Derivative and Functional Principal Component Analysis (FPCA)) for measureing the closeness between curves. Root Mean Square Errors is used for the implementation of this model which is then compared to the independent response method. R program is used for analysing data. Then, when the cov
... Show More
(2)
(1)
Background: Irrigation of the canal system permits removal of residual tissue in the canal anatomy that cannot be reached by instrumentation of the main canals so the aim of this study was to compare and evaluate the efficiency of conventional irrigation system, endoactivator sonic irrigation system,P5 Newtron Satelec passive ultrasonic irrigation and Endovac irrigation system in removing of dentin debris at three levels of root canals and to compare the percentage of dentin debris among the three levels for each irrigation system. Materials and methods: Forty extracted premolars with approximately straight single root canals were randomly distributed into 4 tested groups of 10 teeth each. All canals were prepared with Protaper Universal ha
... Show Moreackground: Escherichia coli is one of the most
important bacterial pathogen that can cause several
disease to human being . In our study we try to
investigate the sensitivity resistance pattern of
Escherichia coli against three antibiotics ( Amikacin,
Nalidixic acid and Cephalexin).
Methods: For this purpose we collected 51 clinical
isolates of Escherichia coli from stool and urine of
outpatient and inpatient patients from different wards
of AL-SADER Teaching Hospital in AL-NAJAF
AL-ASHRAf, IRAQ, and tested by culture and
sensitivity test .
Results: The results appeared that Amikacin show
the highest percentage of sensitivity ( 66.66 % ) ,
while Cephalexin show the lowest percentage of
sensiti
The organic compound imidazole has the chemical formula C3N2H4. Numerous significant biological compounds contain imidazole. The amino acid histidine is the most prevalent. The substituted imidazole derivatives have great potential for treating a variety of systemic fungi infections. Thiourea is an organosulfur compound with the formula SC(NH2)2. It is a reagent in organic synthesis. In this paper, some new imidazole and thiourea derivatives are synthesized, characterized, and studied for their biological activity. These new compounds were synthesized from the starting material terephthalic acid, which was transformed to corresponding ester [I] by the refluxing of diacid with methanol in the presence of H2SO4 as a catalyst, compound [I] con
... Show More
(1)
This study outlines the synthesis of substituted 1,2,4-triazole derivatives through the cyclization reaction of thiourea derivatives. The process begins with the reaction of different halides with KSCN to produce isothiocyanate derivatives. then followed by a reaction with isonicotinic acid hydrazide to yield thioureas (1-6), with a yield rate of (72-88%). Then, compounds (1-6) were treated with alkaline medium 4 N (NaOH) to produced 1,2,4-triazole derivatives (7-12) with a yield (51-69%).The structure of the prepared compounds was characterized using FTIR,1HNMR and 13CNMR spectroscopy. Some of the synthesized compounds were tested for antimicrobial activity when, compound 9 showed strong activity against gram positive bacteria (Sta
... Show More
(1)
A new series of Schiff bases compounds , containing an azomethine linkage was synthesized and expected to be biologically active .The structures of these compounds were identified by IR , Uv/vis spectra , melting points and followed by T.L.C.The biological activity of these compounds was studied
We described herein the synthesized and characterized of new bent and liner core compounds containing thiazolidin-4-one ring[XI-XIII] and [XIV-XVI] respectively. These compounds synthesized by sequence reactions starting from reaction resorcinol or hydroquinone with chloracetyl chloride to yield compounds [I] and [II] ,then the later compounds reactant with 4-hydroxybenzylaldehyde to product dialdehyde compounds [III] and [IV] .The Schiff bases compounds[V-VII] and [VIII-X] synthesized from reaction the compound [III] or [IV] with different aromatic amines, while the bent and liner core mesogens containing thiazolidin-4-one ring [XI-XIII] and [XIV-XVI] synthesized from reaction Schiff bases compounds[V-VII] or [VIII-X] with thioglycolic aci
... Show MoreMetal complexes of Mn(II), Co(II), Ni(II), Cu(II), Cd(II), Zn(II), Hg(II), Pd(II), and Pt(II) with Schiff base ligand (LH) derived from 2,5-dichloroaniline and 2-hydroxy-5-metheylbenzalaldehyde were synthesized and characterized using a variety of spectrophotometric techniques The findings of the spectroscopic analysis indicated that (LH) behaved as a binary coordinating agent to the metal ion by the N and O atoms, and the geometry shape of the complexes was octahedral, with the exception of the Pd and Pt complexes, which had a square planar geometry. Using the DPPH radical scavenging method, we investigated the antimicrobial activity of the compound against Staphylococcus aureus and Escherichia coli, as well as the antifungal activity of t
... Show MoreStick-slip is kind of vibration which associated with drilling operation in around the bottom hole assembly (BHA) due to the small clearance between drill string & the open hole and due to the eccentric rotating of string. This research presents results of specific experimental study that was run by using two types of drilling mud (Fresh water Bentonite & Polymer), with/without Nanoparticle size materials of MgO in various ratios and computes the rheological properties of mud for each concentration [Yield point, plastic viscosity, Av, PH, filter loss (30 min), filter cake, Mud Cake Friction, Friction Factor]. These results then were used to find a clear effects of Nanoparticle drilling mud rheology on stick - slip strength by sev
... Show More
(1)