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.
Abstract
The purpose of this research is to develop a proposed framework for achieving the Integration of the Target Cost and Resource Consumption Accounting Techniques and to show the role they play in reducing products costs and supporting the competitive advantage to cope with contemporary changes. To achieve this goal, the researchers followed the analytical method using the statistical questionnaire as a means of collecting data from the research sample include accounting, administrative, technical, engineering staffs and others. The research sample consists of (56) individuals and for the purpose of conducting statistical analysis of the data and testing hypotheses, the statistical program (SPSS) wa
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(2)
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Some coordination complexes of Co(??), Ni(??), Cu(??), Cd(??) and Hg(??) are reacted in ethanol with Schiff base ligand derived from of 2,4,6- trihydroxybenzophenone and 3-aminophenol using microwave irradiation and then reacted with metal salts in ethanol as a solvent in 1:2 ratio (metal: ligand). The ligand [H4L] is characterized by FTIR, UV-Vis, C.H.N, 1H-NMR,13C-NMR, and mass spectra. The metal complexes are characterized by atomic absorption, infrared spectra, electronic spectra, molar conductance, (C.H.N for Ni(??) complex) and magnetic moment measurements. These measurements indicate that the ligand coordinates with metal (??) ion in a tridentate manner through the nitrogen and oxygen atoms of the ligand, octahedral structures
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(1)
Some coordination complexes of Co(ІІ), Ni(ІІ), Cu(ІІ), Cd(ІІ) and Hg(ІІ) are reacted in ethanol with Schiff base ligand derived from of 2,4,6- trihydroxybenzophenone and 3-aminophenol using microwave irradiation and then reacted with metal salts in ethanol as a solvent in 1:2 ratio (metal: ligand). The ligand [H4L] is characterized by FTIR, UV-Vis, C.H.N, 1H-NMR,13C-NMR, and mass spectra. The metal complexes are characterized by atomic absorption, infrared spectra, electronic spectra, molar conductance, (C.H.N for Ni(ІІ) complex) and magnetic moment measurements. These measurements indicate that the ligand coordinates with metal (ІІ) ion in a tridentate manner through the nitrogen and oxygen atoms of the ligand, octahed
... Show MoreSome coordination complexes of Co(??), Ni(??), Cu(??), Cd(??) and Hg(??) are reacted in ethanol with Schiff base ligand derived from of 2,4,6- trihydroxybenzophenone and 3-aminophenol using microwave irradiation and then reacted with metal salts in ethanol as a solvent in 1:2 ratio (metal: ligand). The ligand [H4L] is characterized by FTIR, UV-Vis, C.H.N, 1H-NMR,13C-NMR, and mass spectra. The metal complexes are characterized by atomic absorption, infrared spectra, electronic spectra, molar conductance, (C.H.N for Ni(??) complex) and magnetic moment measurements. These measurements indicate that the ligand coordinates with metal (??) ion in a tridentate manner through the nitrogen and oxygen atoms of the ligand, octahedral st
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(1)
We have studied in this research litter (Taa) a morphological , sonic indicative and comparative study among four Semitic languages. They are Arabic , Hebrew, Syriac and Akkadian languages . We have divided the research into a number of pivots beginning with an entrance about the letter (Taa) in Semitic languages and the symbols which are used by these languages referring to . Then we have studied (Taa) from sonic side with letters phenomenon (b, g, k, p, t) the six in both Hebrew and Syriac languages . The letter (Taa) is formed one of them and the sonic change that is happening in articulation (Taa) according to sonic rules related to these letters in case of emphasis or in case of neglected (not emphasis). Then we have studied the pro
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The government spending in Iraq and witnessed the changes and developments, especially after 2003, which outweighed consumer spending at the expense of capital expenditure and increased support and diversity of trends towards improving pension conditions for member
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The research aims to diagnose the shortcomings and weaknesses in applying the dimensions of the quality of work life and the extent of their impact on employees’ attitudes and behaviors, and thus their relationship to enhancing their core competencies. The scientific value of the research stems from highlighting the importance of the dimensions of the quality of professional life in improving the productive efficiency of workers in the public sector and raising the level of organizational performance. Because the quality of working life plays an important role in enhancing the core competencies of employees in the public sector, it can also be an incentive or a disincentive for any employee by adapting to the economic and social condition
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