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العنوان
Instrumental Analysis For Determination Of Certain Antibiotics In Pharmaceutical Formulation /
المؤلف
Tolba, Marwa Hamdy Hassan.
هيئة الاعداد
باحث / مروه حمدى حسن طلبه
مشرف / محمد الحسنى الصادق
مشرف / صبحى م. العدل
مناقش / محمد بركه
الموضوع
Cephalosporins- pharmacology. Spectrophotometry- methods.
تاريخ النشر
2014.
عدد الصفحات
160 P. :
اللغة
الإنجليزية
الدرجة
ماجستير
التخصص
العلوم الصيدلية
الناشر
تاريخ الإجازة
1/1/2014
مكان الإجازة
جامعة الزقازيق - كــليـــة الصيدلــــة - Pharmaceutical Chemistry
الفهرس
Only 14 pages are availabe for public view

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Abstract

In this thesis, New HPLC and Spectrophotometric methods were studied for determination of some Cephalosporines and Macrolides drugs in bulk and dosage formsin addition to the optimal method conditionswere studied .
The thesis consists of five main parts:
Part I:-
It describes the theoretical background and literature review of selected drugs on the reported methods for their determination and also chemical structure, physical properties and mode of actions of these cited drugs.
Part II(A):
In this part, an isocratic HPLC method had been developed for rapid simultaneous separation and determination of two cephalosporines with one macrolide including Claritromycin, Cefixime and Cefoperazone in pure form or in presence of some impurities within lese than 5 minutes. Separation was carried out on a Hypersil gold C18 (10um, 100x4.6mm) column. Effect of pH and composition ofmobile phase in addition to flow rates was studied. Beer’s law was obeyed in the range of 1-50 µg/ml for Clarithromycin and Cefixime or 2-50 ug\ml for Cefoperazone. The method was applied for the determination of drugs in both bulk and pharmaceutical forms and results were compared with reference methods.
Part IIB:
In this part, the same isocratic HPLC method had been developed for rapid simultaneous separation and determination of three cephalosporines including Cefepime , Cefotaxime and Cefoperazone within lese than 15 minutes. Separation was carried out on a Hypersil gold C18 (10um, 100x4.6 mm) column. Effect of pH and composition of mobile phase in addition to flow rates was studied. Beer’s law was obeyed in the range of 10-50 µg/ml for all drugs. The method was satisfactory applied for the determination of drugs in both bulk and pharmaceutical forms and results were compared statistically with reference methods.
Part III:
In this part, two simple, accurate and sensitive spectrophotometric methods for determination of Clarithromycin and Clindamycin in bulk and dosage forms using bromocresol purple and bromocresol green dyes are described. Both methods depends on the reaction of the mentioned drugs with either bromocresol purple or bromocresol green dyes to form an ion pair complex could be extracted using organic solvent and measured at 390-397 and 413 nm in case of bromocresol purple and bromocresol green dyes, respectively. Effect of pH, reagent concentration, temperature, solvent, and addition sequence on the absorption was studied. Beer’s law was obeyed in the range of 12-28 µg/ml for Clarithromycin and 8-40 µg/ml for Clindamycin in case of bromocresol purple method and in the range of 4-20 µg/ml for Clarithromycin and 16-32 µg/ml for Clindamycin in case of bromocresol Green method. The proposed methods were applied for determination of Clarithromycin and Clindamycin in pharmaceutical preparations and were validated when the obtained results were compared with reference methods.
Part IV:
In this part, two spectrophotometric methods are described for determination of Clarithromycin , Clindamycin and Cefixime in bulk and pharmaceutical dosage forms using in situ generated bromine as oxidizing agent and either methylene blue or methyl orange as chromogenic agents. Drugs are treated with known excess of bromine and residual unreacted bromine is determined by treating with fixed amount of either methylene blue or methyl orange then measuring absorbances at (666 for Clindamycin and Cefixime nm and 678nm for Clarithromycin) or510 nm respectively. The amount of bromine reacted corresponds to the amount of each drug. Effect of acidity, bromate - bromide volume and time, on the absorption was studied. Calibration curves were linear over ranges of 1.6–4.8 µg.ml-1 for Clindamycin, 3.2–16 µg.ml-1 for Clarithromycin and 0.8-7.2 µg.ml-1 for Cefixime in case of methylene blue, and of 0.8–4 µg.ml-1 for Clindamycin, 6.4–19.2 µg.ml-1 for Clarithromycin and 0.4-2 µg.ml-1in case of methyl orange. The methods were satisfactory applied for the determination of drugs in both bulk and pharmaceutical forms and the results obtained were compared statistically with reference methods.
Part V:
In this part, a simple, accurate and sensitive spectrophotometric method for determination of Cefixime and Cefotaxime in bulk and dosage forms using Ellmans reagent (DTNB) is described. The developed method is based on the alkaline hydrolysis of the studied drugs and subsequent reactions of the resulting hydrolysates with DTNB as a chromogenic reagent giving complex which could be measured at 411 or 417 nm in case of Cefixime and Cefotaxime respectively. Effect of pH, reagent concentration, temperature, NaOH concentration and time of hydrolysis was studied. Beer’s law was obeyed in the range of 0.4-2 µg/ml for Cefixim and 0.8-4 µg/ml for Cefotxime. The proposed methods were applied for determination of both druges in pharmaceutical preparations and were validated and the obtained results were compared with reference methods.