نور
نور

Nouruddin Wageih Sayed Abdelgawad

Ass. Prof.

Basic Informations

C.V
 
Nouruddin Wageih S. Abdelgawad Ali

v PERSONAL DATA

  • Date of birth: November 18th, 1974
  • Place of Birth: Taef, Saudi Arabia
  • Nationality: Egyptian
  • Address: 43 Fakhr Eldawla St., Alerian district, Fayoum, Egypt
  • Cell Phone: +2 0189626757
  • Home Phone:+2 0846300893
  • e-mail address: nour.sayed@pharm.bsu.edu.eg

                          dr.nourali@hotmail.com

 

v ACADEMIC EDUCATIONAL DEGREES

2001-2005      Ph.D., Cairo University, Faculty of Pharmacy, EGYPT

Philosophy doctor degree of pharmaceutical sciences (analytical chemistry). Title of Thesis: "Analytical Study On Some Amide Containing Anti-Inflammatory Drugs"

 

1996-2001     M.Sc., Cairo University, Faculty of Pharmacy, EGYPT

Master degree of pharmaceutical sciences (analytical chemistry). Title of Thesis: "Stability Indicating Methods for The Determination of Some Amide and/or Amine Containing Pharmaceuticals"

 

1991-1996     B.Sc., Cairo University, Faculty of Pharmacy, EGYPT

Bachelor degree of  pharmaceutical sciences

 

v PROFESSIONAL EXPERIENCE (ACADEMIC POSITIONS)

2014-current: Vice dean for education & Students' affairs, Faculty of Pharmacy, Beni-Suef University, , EGYPT

 

2010-current: Ass. Prof. of Analytical Chemistry and Acting Head of Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Beni-Suef University, , EGYPT

 

2005-2010: Lecturer of Analytical Chemistry, Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Beni-Suef University, , EGYPT

 

2001-2005:   Assistant lecturer of Analytical Chemistry, Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Beni-Suef University, , EGYPT

 

1997-2001: Instructor of Analytical Chemistry, Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Beni-Suef University, , EGYPT

 

 

 

v PUBLICATIONS

 

  • Publications abstracted from MSc. & PhD. Theses (5):

 

1.    Nagiba Y. Hasan, Mohamed A.El-Kawy, Badr E.El-Zeany and Nour E. wagieh, “Stability indicating methods for the determination of diloxanide furoate”, Journal of Pharmaceutical and Biomedical Analysis, 28, 187-197, 2002

2.    Nagiba Y. Hasan, Mohamed A.El-Kawy, Badr E.El-Zeany and Nour E. wagieh, “Stability indicating methods for the determination of clozapine”, Journal of Pharmaceutical and Biomedical Analysis, 30, 35-47, 2002.

3.    Nagiba Y. Hasan, Mohamed A.El-Kawy, Badr E.El-Zeany and Nour E. wagieh, “Stability indicating methods for determination of aceclofenac”, IL Farmaco, 58, 91-99, 2003.

4.    Nagiba Y. Hasan, Mohamed A.El-Kawy, Badr E.El-Zeany and Nour E. wagieh, “Stability indicating methods for the determination of piroxicam”, bulletin of faculty of pharmacy. Cairo university, 41(2), 1-10, 2003.

5.    Nagiba Y. Hasan, Mohamed A.El-Kawy, Badr E.El-Zeany and Nour E. wagieh, “Stability indicating methods for the determination of lornoxicam”, bulletin of faculty of pharmacy. Cairo university, 42(3), 1-10, 2004.

  • Publications after appointment as lecturer of analytical chemistry (7):
    1. Nouruddin Wageih Sayed. Application of chemometric methods for simultaneous determination of diosmin and hesperidin in pharmaceutical preparations, Egyptian pharmaceutical Society xxxi conference of pharmaceutical sciences, Cairo, Egypt, 2008.
    2. Nouruddin W. Ali, Mohammed R. Elghobashy, Mohammed Gamal, Mohammed Abdelkawy, Spectrophotometric and spectrofluorimetric methods for simultaneous determination of orphenadrine and paracetamol, 1st international pharmaceutical sciences conference, Faculty of Pharmacy, Tanta University, Tanta, Egypt, 2009.
    3. Nour E. Wagieh, Maha A. Hegazy, M. Abdelkawy, Eglal A. Abdelaleem, Quantitative determination of oxybutynin hydrochloride by spectrophotometry, chemometry and HPTLC in presence of its degradation product and additives in different pharmaceutical dosage forms, Talanta, 80, 2007-2015, 2010.
    4. Nour E. Wagieh, Samah S. Abbas, M. Abdelkawy, Maha M. Abdelrahman. Spectrophotometric and spectrodensitometric determination of triamterene and xipamide in pure form and in pharmaceutical formulation, Drug Testing and Analysis, 2: 113-121, 2010.
    5. Nouruddin W.Ali, Mohammed R.Elghobashy, Mohammed Gamal, Mohammed Abdelkawy. TLC-spectrodensitometric and micro-emulsion RP-HPLC chromatographic methods for determination of orphenadrine and paracetamol, Analytical Chemistry: an Indian Journal, 9(2): 298-304, 2010.
    6. N. W. Ali, S. AbouZid, , A. Nasib, S. Khan, J. Qureshi, M. I. Choudhary. RP-HPLC analysis of withanolides in the flowers, leaves and roots of Withania somnifera, Acta Chromatographica, 22 (3): 473-480, 2010.
    7. Samah S.Abbas, Nour E.Wagieh, M.Abdelkawy, Maha M.Abdelrahman. Spectrophotometric, spectrofluorimetric and HPLC determination of triamterene and xipamide in their binary mixture and in human plasma, Analytical Chemistry: an Indian Journal, accepted 27 february 2010, under publication.

 

  • Publications after appointment as assistant professor of analytical chemistry (32):

1.    Nouruddin Wageih Ali, Mohammed Refaat ELghobashy, Mohammed Gamal Mahmoud, Mohammed Abdelkawy Mohammed, "Spectrophotometric and Spectrofluorimetric methods for determination of racecadotril", Pakistan Journal of Pharmaceutical Sciences, 24 (1), 19-23, 2011.

2.    Samah S. Abbas, Nour E. Wagieh, Mohamed Abdelkawy, Maha M. Abdelrahman, "Simultaneous Determination of Diloxanide Furoate and Metronidazole in presence of Diloxanide furoate Degradation products", Journal of AOAC International, 94 (5),1427-1439, 2011.

3.    Nouruddin W. Ali, Hala E. Zaazaa, M. Abdelkawy and Maimana A. Magdy, "Simultaneous Determination of Paracetamol and Diphenhydramine Hydrochloride in Presence of Paracetamol Degradation Product", Pharmaceutica Analytica Acta, 2 (9), (2011)

4.    Nouruddin W. Ali, Nada S. Abdelwahab, M. Abdelkawy, Amal A. Emam, “Spectrofluorimetric determination of Diacerin in presence of its metabolite", presented at The 32nd International Conference of Pharmaceutical Sciences, Egyptian Pharmaceutical Society, Cairo, Egypt(2011)

5.    Nouruddin W. Ali, Nada S. Abdelwahab, M. Abdelkawy, Amal A. Emam, “Validated Spectrophotometric and spectrodensitometric methods for determination of some analgesic drugs in different dosage forms", presented at The 32nd International Conference of Pharmaceutical Sciences, Egyptian Pharmaceutical Society, Cairo, Egypt(2011)

6.    Nouruddin W. Ali, Nada S. Abdelwahab, Hamed M. Elfatatry, Weam M. Osman, “Development and validation of different spectrophotometric, chromatographic methods for determination of two hypouricemic drugs in their combined dosage form", presented at The 32nd International Conference of Pharmaceutical Sciences, Egyptian Pharmaceutical Society, Cairo, Egypt(2011)

7.    Nouruddin W. Ali, Nada S. Abdelwahab, Weam M. Osman, “Validated Spectrophotometric, TLC densitometric and RP-HPLC methods for determination of two antidiabetic drugs in their combined dosage form", presented at The 32nd International Conference of Pharmaceutical Sciences, Egyptian Pharmaceutical Society, Cairo, Egypt(2011)

8.    Nouruddin W. Ali, Maha A. Hegazy, M. Abdelkawy, Eglal A. Abdelaleem, “Simultaneous determination of Methocarbamol and its related substance(Guaifenesin) in two ternary mixtures with Ibuprofen and Diclofenac Potassium by HPTLC spectrodensitometric method", Journal of Planar Chromatography, 25 (2), 150-155, (2012)

9.    Nouruddin W. Ali, Samah Sayed Abbas, Hala El-Sayed Zaazaa, Maha Mohamed Abdelrahman, Mohamed Abdelkawy, “Validated stability indicating methods for determination of nitazoxanide in presence of its degradation products", Journal of Pharmaceutical Analysis, 2 (2), 105-116, (2012)

10. Nouruddin W. Ali, Maha A. Hegazy, M. Abdelkawy, Eglal A. Abdelaleem, “Simultaneous determination of Methocarbamol and Ibuprofen or Diclofenac Potassium using mean centering of of the ratio spectra method", Acta Pharmaceutica, 62, 191-200, (2012)

11. Nouruddin W. Ali, Nada S. Abdelwahab, Marco M. Zaki and M. Abdelkawy, “Validated chromatographic methods for simultaneous determination of Amlodipine Besylate and Perindopril Arginine in binary mixtures and in pharmaceutical dosage form", Journal of Chromatography and Separation Techniques , 3(4), (2012)

12. Nouruddin W. Ali, Nada S. Abdelwahab, M. Abdelkawy and Aml A. Emam, “Validated spectrophotometric and spectrodensitometric methods for determination of a ternary mixture of analgesic drugs in different dosage forms", Bulletin of Faculty of Pharmacy, Cairo University, 50, 99-109, (2012)

13. Nouruddin W. Ali, Mohammed Gamal and Mohammed Abdelkawy, “Simultaneous determination of Hyoscine Butyl Bromide and Dipyrone in their binary mixture by RP-HPLC method", IOSR Journal of Pharmacy and Biological Sciences, 3(5), 29-36, (2012)

14. Nouruddin W. Ali, Hala A. Zaazaa, M. Abdelkawy and Maimana A. Magdy, “Simultaneous HPTLC and RP-HPLC methods for determination of Bumadizone in the presence of its alkaline induced degradation product", Biomedical Chromatography, 26, 1143-1149, (2012)

15. Nouruddin W. Ali, Maha A. Hegazy, M. Abdelkawy and Eglal A. Abdelaleem, "Simultaneous determination of Methocarbamol and its related substance (Guaifenesin) in two ternary mixtures with Ibuprofen and Diclofenac potassium by RP-HPLC method", Journal of liquid Chromatography and Related Technologies, 35(16), 2229-2242, (2012)

16. Safa'a M. Riad and Nouruddin W.Ali, "water hyacinth roots as economic potential biomass for the removal of organic pollutants in waste water via application of coated wire electrodes", Analytical & Bioanalytical Electrochemistry, 4(5), 480-497, (2012)

17. Nouruddin W. Ali, Mohammed Gamal and Mohammed Abdelkawy, “Simultaneous determination of Hyoscine Butyl Bromide and Dipyrone in their binary mixture by RP-TLC spectrodensitometric method", International Journal of Chemical and Analytical Science, 3(10), 1578-1582, (2012)

18. Safa'a M. Riad and Nouruddin W. Ali, "Novel Conductometric procedures for Cilostazol Determination in Pharmaceutical Formulations, its degradation product and plasma", International Journal of Chemical and Analytical Sciences, 3(12), 1629-1633, (2012)

19. Nouruddin W. Ali, Nada S. Abdelwahab, Badr A. El-Zeiny and Salwa I. Tohamy, “Stability indicating TLC-densitometric method for determination of chlorpropamide", Journal of Liquid Chromatography & Related Technologies , 36(11), 1575-1585, (2013)

20. Nouruddin W. Ali, Mohammed Gamal and Mohammed Abdelkawy, "Simultaneous determination of hyoscine N-butyl bromide and paracetamol by RP-TLC spectrodensitometric method", British Journal of Pharmaceutical Research, 3(3), 472-484, 2013

21. Nouruddin W. Ali, Maha Ahmad Hegazy, Mohammed Abdelkawy, “Simultaneous determination of naphazoline hydrochloride, chlorpheniramine maleate and methylene blue in their ternary mixture" Pakistan Journal of Pharmaceutical Science, 26(3), 641-648, (2013)

22. Nouruddin W. Ali, M. Abdelkawy and Nessreen S. Abdelhamid, “Simultaneous determination of Paracetamol and diphenhydramine hydrochloride mixture in the presence of their degradation products", IOSR Journal of Pharmacy and Biological Sciences, 6(5), (2013)

23. Hala E. Zaazaa, Nouruddin W. Ali, Maimana A.Magdy, Mohamed Abdelkawy, "Stability indicating spectrophotometric methods for determination of bumadizone in the presence of its alkaline degradation product", Drug Invention Today, 5, 139-147, (2013)

24. Nour W. Sayed, Maha A. Hegazy, Eglal A. Abdelaleem, M. Abdelkawy and Rehab M. Abdelfatah, “Stability indicating spectrophotometric and spectrodensitometric methods for determination of calcium dobesilate in the presence of its impurity and/or degradation product, International Journal of Pharmacy and Pharmaceutical Sciences, 5(3), (2013)

25. Nouruddin W. Ali, Mohammed Gamal and Mohammed Abdelkawy , “chromatographic methods for simultaneous determination of diiodohydroxyquinoline and metronidazole in their binary mixture", Pakistan Journal of Pharmaceutical Science,  26(5), 865-871, (2013)

26. Safa'a M. Riad and Nouruddin W. Ali, “Novel Poly(vinyl chloride) matrix membrane sensors for determination of Cilostazol in presence of its degradation product and in plasma", Analytical & Bioanalytical Electrochemistry 5(5), 622-634, (2013)

27. Nouruddin W. Ali, Nada S. Abdelwahab, M. Abdelkawy and Aml A. Emam, "Validated stability indicating TLC-densitometric method for the determination of diacerein", Journal of Chromatographic Science, 52, 5-11, (2014)

28. M. H. HETTA, H. F. ALY, N. W. ALI, "Estimation of resveratrol content in peanut pericarp and its relation to the in vitro inhibitory activity on carbohydrate metabolizing enzymes", Pharmazie, 69, 92-95, (2014)

29. Hala E. Zaazaa, Maha M. Abdelrahman, Nouruddin W. Ali, Maimana A. Magdy, M. Abdelkawy, "Kinetic study and mechanism of niclosamide degradation", Spectrochimica Acta Part A:Molecular and Biomolecular Spectroscopy, 132, 655-662, (2014)

30. Eglal A. Abdelaleem, Maha A. Hegazy, Nour W. sayed, M. Abdelkawy, Rehab M. Abdelfatah, "Novel spectrophotometric determination of flumethasone pivalate and clioquinol in their binary mixture and pharmaceutical formulation", Spectrochimica Acta Part A:Molecular and Biomolecular Spectroscopy, 136, 707-713, (2015)

31. Nada S. Abdelwahab, Nouruddin W. Ali, Marko M. Zaki, M. Abdelkawy, "Validated Chromatographic Methods for Simultaneous Determination of Tolfenamic acid and its major impurities", Journal of Chromatographic Science, 53, 484-491, (2015)

32. Nouruddin W. Ali, Mohammed Gamal, Mohammed Abdelkawy, "Simultaneous determination of hyoscine N-butyl bromide and paracetamol in their binary mixture by RP-HPLC method", Arabian Journal of Chemistry, in press corrected proof, available on line 2014.

 

 

 

 

 

 

 

 

v CERTIFICATES AND COURSES

  • "E-learning Content Development ", the American University in Cairo, Cairo, Egypt, (2005).
  • -"Pharmaceutical analysis: assay development and validation made easy", Saudi Pharmaceutical Society, Riyadh, Kingdom of Saudi Arabia, (2007).
  • "International Scientific Publishing", FLDP center, Beni-Suef University, Beni-Suef, Egypt, (2008).
  • "Use of Technology in Education", FLDP center, Beni-Suef University, Beni-Suef, Egypt, (2008).
  • "Nano science and nanotechnology", faculty of science, Beni-Suef University, Beni-Suef, Egypt, (2010).
  • "Preparation of scientific conferences", ", FLDP center, Beni-Suef University, Beni-Suef, Egypt, (2010).
  • "Radio applications of chromatographic analysis (basis-types-applications)", RMECRIAC center, Cairo, Egypt, (2010).
  • "Ethics in Scientific Research", FLDC center, Beni-Suef University, Beni-Suef, Egypt, (2011).
  • "Financial & legal aspects in university affairs", FLDC center, Beni-Suef University, Beni-Suef, Egypt, (2011).
  • "Student evaluation and examination techniques", FLDC center, Beni-Suef University, Beni-Suef , Egypt, (2014).

 

v CONFERENCES

  • The 7th international Saudi Pharmaceutical Conference, Saudi Pharmaceutical Society, Riyadh, Kingdom of Saudi Arabia, (2007).
  • The First International Pharmacy Conference, Saudi German Hospital, Riyadh, Kingdom of Saudi Arabia, (2008).
  • The 31th International Conference of Pharmaceutical Sciences, Egyptian Pharmaceutical Society, Cairo, Egypt, (2008).  
  • The Informational Conference on Mechanisms of delivering and Application of Quality culture and concepts, Performance Appraisal and Quality Assurance Unit, Faculty of Pharmacy, Cairo university,  Cairo, Egypt, (2008).  
  • The first international conference of the national authority for quality assurance and accreditation of education, Cairo, Egypt, (2008).
  • The first International Pharmaceutical Sciences Conference, Faculty of Pharmacy, Tanta University, Tanta, Egypt, (2009).
  • The 2nd scientific conference of faculty of pharmacy –Cairo university, Cairo, Egypt, (2010)
  • The International Summit Forum of Biotechnological & Medical Industry- Shijiazhuang, Hebei Province, China (2011)
  • International Conference & Exhibition on Pharmaceutical Biotechnology"- Hyderabad, India (2011)
  • Egyptian Chemical Conference "Celebrating the International Year of Chemistry", Cairo, Egypt (2011)
  • The 32nd International Conference of Pharmaceutical Sciences, Egyptian Pharmaceutical Society, Cairo, Egypt, (2011)
  • FUE International Conference of Pharmaceutical Technologies, Future University, Cairo, Egypt, (2012).
  • FUE International Conference of Pharmaceutical Sciences, Future University, Cairo, Egypt, (2013).

 

 

v TEACHING EXPERIENCE

  • Teaching general chemistry, physical chemistry, analytical chemistry, instrumental analysis and quality assurance and control courses for undergraduate and postgraduate students.
  • Teaching relevant subjects for undergraduate and postgraduate students.
  • Assisting young researches concerning work with different analytical techniques.
  • Participation in different activities related to educational development including curricula establishing and development for pharmacy students.
  • Participation in different activities related to research development such as participation in conferences and seminars, supervising M.Sc. and Ph.D. students ….etc.

v RESEARCH AREAS OF INTEREST

  • Utilization of different analytical techniques including spectroscopic methods, HPLC, TLC and densitometry chromatographic methods.
  • Establishment of stability indicating methods for different pharmaceuticals
  • Development of analytical methods for determination of pharmaceutical drugs in biological fluids.
  • Impurity profiling of pharmaceutical drugs.
  • Use of computer programs in delivering scientific materials to students

 

 

 

v PROFESSIONAL MEMBERSHIPS

  • AOAC (American Organization for Analytical Chemists) International
  • Egyptian Syndicate for Pharmacists
  • Egyptian Pharmaceutical Scientific Society
  • Beni-Sueif University Staff Association Club
  • Cairo University Staff Association Club 

 

v Recognitions and Awards

  • Who's Who in the world 2012 book
  • Beni-Suef University Best Research Award 2012
  • Silver medal from Egyptian Pharmacists Syndicate  for best achievement 2012  

 


C.V PDF

Master Title

STABILITY INDICATING METHODS FOR THE DETERMINATION OF SOME AMIDE AND /OR AMINE CONTAINING PHARMACEUTICALS

Master Abstract

PREFACE Most pharmaceutical compounds are subjected to degradation accompanied with partial, or even complete loss of pharmacological activity. Stability indicating methods are developed for determination of the extent of drug degradation. A stability indicating method is defined as any method that affords selective determination of the intact drug in presence of its degradation product(s). The object of the present work is to develop simple, efficient and selective methods for the quantitative determination of the intact molecules of the three studied drugs namely, aceclofenac (AC), clozapine (CL), diloxanide furoate (DF), which can be adopted for their stability studies. The thesis comprises four parts: PART I: GENERAL INTRODUCTION In this part, a brief idea about sources of drugs degradation and the theoretical background for stability indicating methods. PART II: Stability indicating methods for the determination of aceclofenac This part comprises: 1- Literature review about structure, properties, pharmacology and the reported methods for analysis of aceclofenac. I 2-Experimental study, dealing with the determination of AC in presence of its degradation product by spectrophotometric, densitometric and high-performance liquid chromatographic (HPLC) methods. PART III:Stability indicating method for the determination of clozapine This part comprises: 1- Literature review about structure, properties, pharmacology and the reported methods for analysis of clozapine. 2-Experimental study, concerned with the determination of CL in presence of its degradation product by spectrophotometric, densitometric and high-performance liquid chromatographic (HPLC) methods. PART IV: Stability indicating method for the determination of diloxanide furoate This part comprises: 1- Literature review about structure, properties, pharmacology and the reported methods for analysis of diloxanide furoate. 2-Experimental study, about the determination of DF in presence of its degradation products using spectrophotometric, densitometric and high-performance liquid chromatographic (HPLC) methods. This thesis further comprises 122 references and ends with an arabic summary. II I.1. Concepts in drug stability Most drugs are subject to some forms of decomposition, including physical, chemical and microbiological changes that may lead to partial or complete loss of the desired pharmacological activity or even to the production of harmful decomposition products (1). Drug degradation may result either from hydrolysis or oxidation. Drugs may also lose their activity due to isomerisation or photochemical decomposition (1-4) . I.2. Sources of drugs degradation 1- Temperature: Thermal effects are involved in almost all chemical reactions. High temperature results in rapid degradation while cooling diminishes it. For example storing ?-lactam penicillins in a refrigerator reduces the hydrolysis rate by 90% of that at room temperature (3) . 2- Hydrolysis: The most likely cause of drug instability is hydrolysis, which is due to the presence of hydrolysable groups such as ester or amide groups. Procaine, atropine, aspirin, pilocarpine, penicillins, cephalosporins, benzodiazepines, and tetracyclines as well as the three studied drugs in this thesis AC, CL and DI are examples of drugs suffering from hydrolytic decomposition (1-3,5) . -1- 3-Solvolysis: When the reacting solvent is no longer water, then the breakdown is termed “ solvolysis”. Furthermore, the definition can be extended to include any change in solvent polarity and resulting into increased ionic strength. For example, phenobarbitone is considerably more stable in preparations containing water-miscible solvents whereas acetylsalicylic acid, which undergoes extensive hydrolysis, is degraded further by aqueous solvents (3). 4-Oxidation: Oxidative degradation is a major cause of drug instability. Phenolic compounds (e.g. morphine and phenyl ephedrine), catecholamines (e.g. dopamine and adrenaline), steroids (e.g. prednisolone and hydrocortisone), antibiotics (e.g. streptomycin and neomycin), vitamins (e.g. vitamins A, D and E) and other similar compounds are greatly affected by oxidation (1,2). 5- Photolysis: Oxidation and, to some extent hydrolysis are often catalyzed by light. Photodegradation is greatly dependent on both the intensity and wavelength of light and is usually mediated by free radicals. Therefore, protection from light is essential in case of photosensitive drugs. Among these drugs are benzodiazepines, catecholamines, corticosteroides, phenothiazines and most of the vitamins (1,3) . -2- 6-Isomerisation: It is the process of conversion of a drug into its optical or geometrical isomers. Since various isomers of a drug are frequently of different activities, such conversion may be regarded as a form of degradation (1). For example, the appreciable loss of activity of adrenaline solutions at lower pH has been attributed to racemization of the active (L)- form into its less active isomer (6). Tetracyclines undergo epimerization under acidic conditions to give 4-epi-tetracyclines which posses much less activities than the natural isomers (7). I.3. Stability indicating methods of analysis The method used to indicate the stability of a compound should be sufficiently sensitive and selective to determine quantitatively the intact drug in the presence of its degradation products (2,8). During drug formulation, the active ingredient is diluted or dispersed in pharmacologically inert excipients which are not necessarily chemically inert. Thus the analytical problem is far more complex and stability is much more difficult to predict than in case of pure active ingredients (2). A pharmaceutical analytical chemist has, therefore, to develop selective methods that, not only avoid interferences by other coformulated compounds, but also exclude degradation products. -3- The following approaches have been proposed for developing a stability indicating method: [a] Functional group approach: Functional group analysis is greatly concerned with stability indicating methods. A functional group assay is one that is selective for a particular structural feature in a molecule and is considered as a stability indicating one, if such a feature disappears after decomposition (9) , for example hydroxamic acid method is frequently used for the determination of penicillins via the ?-lactam ring. Further, if the functional group dealt with is, at the same time, the "pharmacologically active group ", the chemical method would also determine the " activity " of the drug (10-12). [b] Combination of separation and measurement operations: In several cases a preliminary separation step is carried out before measurement. This is usually done either by using solvent extraction or chromatographic separation (2,14). [b-1] Solvent extraction: The selectivity of direct spectrophotometry has been improved through preliminary separation techniques, such as organic solvent extraction of the amine formed by the hydrolysis of atropine in alkaline medium, followed by UV measurement in acid medium (2) . Also, the direct spectrophotometric determination of Clorazepate dipotassium via N-desmethyldiazepam (15), or via its final degradation products (16), were accomplished through preliminary organic solvent extractions. -4- [b-2] Chromatographic separation: Separation was also affected by TLC followed by UV spectrophotometric determination of chloramphenicol and its palmitate in presence of their degradates (17) and in studying their hydrolysis, kinetics (18). Similarly, the colorimetric determinations of streptomycin and its dihydride (19,20) in pharmaceutical preparations were carried out after chromatographic separations. Also secnidazole was determined in presence of its degradates using densitometry after separation on a TLC plate (21) . [C] Determination of the intact drug in presence of its degradate without separation This can be done by using suitable and selective methods, including: [C.1] Spectroscopic methods: C.1.a. UV-Visible spectrophotometric methods – Direct UV-Visible spectrophotometry has been widely used in pharmaceutical analysis to study decomposition mechanisms but, generally, it lacks sensitivity. However, Amer et al (22) used the orthogonal functions to determine intact nystatin selectively in presence of its degradation products, by direct UV-measurements. Several stability indicating colorimetric methods have been reported. For example, the micro-colorimetric determination of thiamine through its precipitation with a special iodobismuthic acid reagent without any interference from its hydrolytic products (23). Different reagents were also used to quantitate some H2-antagonists in presence of their decomposition products by colorimetric procedures (24). In addition, the acid-dye technique -5- has been reported for the determination of nizatidine in presence of its degradate (25). Also the basic dye "neutral red " was used for the determination of ibuprofen in presence of its degradation product (26) . Derivative spectrophotometry has become a well established technique for the analysis of drugs in mixtures and formulations. The main advantage of this technique is the improvement of resolution of the overlapping absorption bands and, consequently, the accuracy and precision of absorption spectra methods. Clorazepate dipotassium (16), nizatidine (24) , carbamazepine (27) , secnidazole (21) and some cephalosporins (28) were determined in presence of their degradation products by derivative spectrophotometry. A new spectrophotometric method for resolving binary mixtures was proposed by Salinas et al (29), based on the simultaneous use of the first derivatives of the ratio spectra of substances with overlapping spectra and is termed ratio-spectra first derivative spectrophotometry (RSD1). An RSD1 method for the determination of noramidopyrine methane sulfonate sodium salt, pitophenon hydrochloride and fenpiverine bromide in pharmaceuticals was developed by Morelli (30). Nevin et al (31) described an RSD1 method for the simultaneous determination of hydrochlorothiazide and amiloride hydrochloride in sugar coated tablets. Also, Özkan et al (32) used RSD1 spectrophotometry for the simultaneous determination of two-component mixtures in pharmaceutical formulations containing chlordiazepoxide. Direct UV spectrophotometry is particularly useful in case of compounds whose absorption spectra are affected by changing pH .The decomposition of iodoxuridine (33) and phenobarbitone (34) have been determined by measuring -6- their absorbances at different pH. Difference spectrophotometry was also used for the determination of azathioprine in presence of its degradation product (35). C.1.b. Fluorimetric methods - Spectrofluorimetric methods are used when great sensitivity is required. Tetracycline and its degradate, (anhydrotetracycline) were separately determined using fluorimetry (36). C.1.c.NMR-spectroscopic methods -Although NMR-spectroscopic methods was applied either qualitatively or quantitatively as it offers specificity along with simplicity of operation, yet, it lacks sensitivity and precision. It has few applications in stability evaluation such as the determination of clonazepam in presence of its degradation products (37). [C.2] Electrochemical methods: Polarographic techniques have been adopted for the analysis of ethacrynic acid in presence of its decomposition products (38) .A polarographic investigation was used to follow the acid-base hydrolysis and ?-lactamase degradation of several cephalosporins (39). Other electrochemical methods include amperometric titration of ampicillin through its hydrolysate, penicillamine (40), and voltametric assay of bromazepam degradate, (2-amino-5-bromobenzoylpyridine) (41). [C.3] Titrimetric methods: A simple, titremetric, stability indicating method was adopted for the determination of nitromin via its pharmacologically active functional group (10). Said et al (23) developed a titrimetric method for the determination of thiamine in presence of its hydrolytic product. -7- [C.4] Chromatographic methods: Due to their high separation power, different chromatographic techniques were widely applied in stability indicating procedures, including paper (42) , TLC (43,44) , column (45,46) and gas liquid chromatography (47,48) . High-performance liquid chromatography (HPLC) combines the excellent separation properties of column chromatography with spectrophotometry and is considered one of the most useful and applicable selective analytical techniques for the determination of numerous drugs in presence of their degradation products (49-52). In this thesis five different selective methods, namely, Derivative spectrophotometry, Ratio-spectra first derivative spectrophotometry, pH-induced difference spectrophotometry, Densitometry and High performance liquid chromatography (HPLC), were adopted for the determination of intact aceclofenac, clozapine and diloxanide furoate in presence of their degradation products. The suggested methods are simple, accurate, selective and sensitive. Application of the proposed methods to the analysis of the aforementioned three drugs in their pharmaceutical formulations shows that neither the excipients usually formulated in these market preparations nor the degradation products interfere with the determinations. -8-

Master Abstract PDF

PHD Title

ANALYSIS OF SOME AMIDE CONTAINING NON-STEROIDAL ANTI-INFLAMMATORY DRUGS

PHD Abstract

PHD Abstract PDF

All rights reserved ©Nouruddin Wageih Sayed Abdelgawad