Author name:
اوس مسير نجرس خليل الجوعاني
Supervisor name:
معاذ عبد الله نجم الحجار
University location:
Mosul
Key words:
- lisinopril
- spectrophotometric methods
- F test
- t test
- dopamine
- mesalazine
- British Pharmacopeia
Abstract:
The thesis included four chapters: Chapter One: It included a general introduction for pharmaceutical compounds (lisinopril dihydrate, mesalazine, and dopamine dihydrochloride), the extent of their importance, their therapeutic role, and the scientific name. It also explained the chemical form and their physical and chemical properties, in addition to the aim of the research. Chapter Two: The second chapter reviewed previous studies on the pharmaceutical compounds under study for four main methods. The standard methods were intended for comparison with the proposed method, in addition to spectroscopic methods, chromatographic methods, and electrochemical methods, which were reviewed according to the chronological order of the studies obtained. Chapter Three: It includes the practical part, which shows the purity of materials and methods of preparing solutions for the chemical compounds used, in addition to showing the place of obtaining pharmaceutical preparations and methods of preparing their solutions for the purpose of study, and the devices used in the preparation, measurement and determination processes. Chapter Four: It included a review of the results obtained from determining the optimal conditions and their application to pharmaceutical preparations and their discussion. The chapter was divided into three parts. The first part included two sides, the first of which reviewed the results of the indirect spectroscopic determination of lisinopril dihydrate by means of bleaching dye reaction resulting from the reaction of lisinopril dihydrate with N. - Bromosuccinimide as an oxidizing agent in an acidic medium, then reacting the excess of the oxidizing agent with the indigo-carmine dye, which works to bleaching dye. All the factors that affected the reaction were studied, namely: the amount and type of acid used to provide the acidic medium, as well as the optimal amount of dye for use. The times required for complete oxidation and the time required for the color of the dye to fade were also studied. After establishing this, the determination range was determined based on Beer’s law, and it was 5-60 µg.ml-1. The value of the Molar absorptivity was 0.18 x 104 L.mol-1.cm-1 and the Sandell's sensitivity was 0.232 µg.cm-2, which indicates that the method has good sensitivity. The average percentage of recovery and the relative standard deviation were 99.75% and 1.527, respectively, which It indicates that the method had good accuracy and precision. The second side, determination of lisinopril was through the relative derivation of the lisinopril pharmaceutical preparation combined with the amlodipine compound, using the fourth derivative spectrum method, and by determining the appropriate wavelengths in estimating the pharmaceutical preparations incorporated into the pharmaceutical preparation at the same time. It gave flexibility in estimating the two compounds simultaneously by providing three longer wavelengths for lisinopril dihydrate (203, 207, 231 nm) and three longer wavelengths for amlodipine (215, 254, 277 nm). Good accuracy and compatibility were available at each wavelength, in addition to being unaffected by the presence of Excipients and additives for the pharmaceutical preparation. The second part refers to the part of the mesalazine drug compound. The first side was based on the determination of mesalazine using the nitration and coupling reactions with DHNP through the formation of the diazonium salt of mesalazine by taking equal concentrations of the mesalazine compound and sodium nitrite (6.530×10-4 mol.L-1) and adding 3 ml of concentrated hydrochloric acid (11.8M) gradually, stirring continuously, and cooling in an ice bath. Then studied the times required to reach a complete reaction of dizonium salt, The value of the Molar absorptivity was 1.58×104 L.mol-1.cm-1 and the Sandell's sensitivity was 0.0082 µg.cm-2. The average percentage of recovery and the relative standard deviation were 99.2% and 0.029 respectively, As for the second side of the determination of the mesalazine compound, it relied on the reaction of complex formation with one of the iron salts, represented by iron(III) sulphate , it gave linearity Between 2.5-30 µg.ml-1, accuracy represented by average recovery which was at 99.33%, and precision represented by the relative standard deviation, which was 3.29, and the Molar absorptivity value and Sandell's sensitivity were solved as follows: 2.78×103 Lmol-1.cm-1 and 0.054 µg.cm-2, which represent sensitivity method. The third part was about the determination of dopamine hydrochloride and was estimated in two ways. The first relied on the oxidation reaction and coupling with 5-amino salicylic acid (mesalazine) as a coupling agent in a basic medium of sodium hydroxide in the presence of sodium persulfate (Na2S2O8) as an oxidizing agent. The method gave good results in terms of extent The estimate was 2.5-31.25 µg.ml-1. With good sensitivity, by finding the value of the Molar absorptivity and Sandell's sensitivity were solved as follows: 0.55×104 l.mol-1.cm-1 and 0.034 µg.cm-2. In addition to the average recovery of 100.93% and the relative standard deviation of 1.13, which represent the accuracy and precision of the method. As for the second method, which relied on indirect determination through a redox reaction, using yttrium ion as an oxidizing agent and 1.10-phenanthroline as a reagent. The reaction was conducted in an acidic medium provided by hydrochloric acid. The method was successfully applied for determination within a linear range between 0.5-10 µg.ml-1 and good sensitivity was determined by calculating the values of the Molar absorptivity and the Sandell's sensitivity which were 1.44 ×104 lmol-1.cm-1 and 0.0131 µg.cm-2, with an average recovery of 99.58% and a relative standard deviation of 0.83, which represent accuracy and precision , which it was good .
