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العنوان
Chromatographic And Spectrometric Analysis of Some Fluoroquinolones /
المؤلف
Ahmde, Fatma Al-Zahraa Moustafa Abdel-Aal.
هيئة الاعداد
باحث / فاطمه الزهراء مصطفى عبد العال احمد
مشرف / جمال احمد صالح
مناقش / محى خالد شرف الدين
مناقش / محمد وفاء ابراهيم
الموضوع
Analytical Chemistry.
تاريخ النشر
2012.
عدد الصفحات
239 P. ;
اللغة
الإنجليزية
الدرجة
ماجستير
التخصص
الصيدلة ، علم السموم والصيدلانيات (المتنوعة)
الناشر
تاريخ الإجازة
26/6/2012
مكان الإجازة
جامعة أسيوط - كلية الصيدلة - (Pharmaceutical Analytical Chemistry)
الفهرس
Only 14 pages are availabe for public view

from 272

from 272

Abstract

The presented thesis is concerned with the densitometric and chemiluminescence determination of some fluoroquinolones (FQs) namely: Ciprofloxacin (Cip.), Gatifloxacin (Gat.), Levofloxacin (Lev.), Lomefloxacin hydrochloride (Lom.HCl), Norfloxacin (Nor.), Ofloxacin (Ofl.) and Sparfloxacin (Spr.). It comprises five main parts:-
Part I:
Includes the general introduction about FQs that provides general informations about mechanism of action, adverse effects, chemistry, medicinal importance and physico-chemical and pharmacokinetic properties of FQs.
Part II:
Includes a literature review providing official methods included in different pharmacopoeias and reported methods including microbiological, titrimetric, spectrometric, separation and electrochemical methods for determination of FQs.
Part III:
This part consists of two chapters:
Chapter I:
Concerns with development of a simple, rapid, accurate, precise and sensitive UV-spectrodensitometric method for determination of some FQs including (Cip., Gat., Lev., Lom.HCl, Ofl. and Spr.) in their bulk forms and different pharmaceutical dosage forms measured as follows: 278 nm for Cip., 290 nm for Lom.HCl, 292 nm for Gat. and Spr. and 296 nm for Lev. and Ofl. after optimization of mobile phase and reaching to the optimum one (Butanol: methanol: 33% ammonia, 8: 1: 3.5, v/v/v). Beer’s law was obeyed for all studied FQs in concentration ranges of 7.5-150 ng/band for Gat., Ofl. and Spr., 15-150 ng/band for Lom.HCl, 7.5-120 ng/band for Cip. and 7.5-90 ng/band for Lev. The detection and quantitation limits for the studied FQs were not more than 2.98 and 9.04 ng/band, respectively. The method was successfully applied to the analysis of the studied drugs in pure forms and in their pharmaceutical dosage forms (tablets, i.v. infusions and eye DROPs). Results were compared with those obtained from official and reported methods. The t- and F-values were calculated and compared with the theoretical values, indicating high accuracy and good precision of the proposed method.
Chapter II:
Concerns to development of a simple, rapid, accurate, precise, sensitive, specific and selective UV-spectrodensitometric stability indicating and kinetic study for determination of Nor. in its pure form and pharmaceutical dosage forms and measured at 282 nm.
Beer’s law was obeyed for Nor. in a concentration range of 6-150 ng/band. The detection and quantitation limits for Nor. were 1.01 and 3.06 ng/band, respectively. The method was successfully applied to the analysis of Nor. in its pure form and different pharmaceutical dosage forms. Results were compared with those obtained from the official method. The t- and F-values were calculated and compared with the theoretical values, indicating high accuracy and good precision of the proposed method.
The method is considerd also selective and specific as it is able to determine Nor. in the presence of co-formulated compounds (ex: tinidazole in Conaz tablets) and in the presence of its degradation products. The method introduced also a stability indicating study after forced acid- and base-degradation of Nor. in 2M HCl and 2M NaOH, respectively by adjusting heating mantle at 150 ºC for 32 hours. The method includes also study for stability of Nor. in solution. The method provided also a kinetic study for Nor. after its forced degradation and calculated the 1st order rate constant (Kobs) and the half life time (t1/2) for acid and base degradation.
Part IV:
Includes development of a simple, rapid, accurate, precise and sensitive chemiluminescence method for determination of seven FQs namely: Cip., Gat., Lev., Lom.HCl, Nor., Ofl. and Spr. in their bulk forms and different pharmaceutical dosage forms. The method is based on the inhibition effect of the studied drugs on the chemiluminescence emission intensity of N-bromosuccinimide (NBS)-luminol system and measured at 425 nm.
Investigations were carried out to study all variables affecting the reaction conditions. Beer’s law was obeyed for all studied FQs in concentration ranges of 50 to 400 ng/ml for Cip. and Nor., 50 to 600 ng/ml for Gat., Lom.HCl and Spr. and 25 to 400 ng/ml for Lev. and Ofl. The detection and quantitation limits for the studied FQs were not more than 4.88 and 14.80 ng, respectively. The method was suucessfully applied to the analysis of the studied drugs in pure forms and in their pharmaceutical dosage forms. Results were compared with those obtained from official and reported methods. The t- and F-values were calculated and compared with the theoretical values, indicating high accuracy and good precision of the proposed method.
The method introduced a stability indicating and a kinetic study for Nor. as an example after forced acid and base degradation in 2M HCl and 2M NaOH adjusting heating mantle at 150 ºC till 32 hrs. The content remained after degradation was calculated and the 1st order rate constant (Kobs) and t1/2 were calculated for acid and base degradation.
Part V:
A single and multiple regression analysis were made between slope of the standard curves of the studied drugs using the proposed TLC-densitometric method (expressed as a sensitivity parameter) and different electronic, biological and topographical parameters. It was found that summation of these parameters have additive effect on each other in the correlation with the sensitivity of the proposed method giving good correlation.
The importance of these correlations between these parameters and the sensitivity parameter comes from the importance of these parameters and their influence on the biological activity of the studied drugs.
N.B
• Part of the analytical review (part II) was accepted for publication in the Journal of Liquid Chromatography & Related Technologies.
• Part III chapter 1 was accepted for presentation as a poster at the Assiut University 8th International Pharmaceutical Science Conference, Faculty of Pharmacy, Assiut, Egypt, March 12-13, 2012, page 101.
• Part III chapter 2 was accepted for publication in the Journal of Liquid Chromatography & Related Technologies.