Basic Informations
C.V
CURRICULUM VITAE
Name: Eglal Abdelhameed
Abdelaleem
Nationality:
Egyptian Date of Birth:
Noember 12, 1981.
Current Position: lecturer
of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Beni-Suef
University, Beni-Suef, Egypt.
Home Address: Ehnasia,
Beni-Suef, Egypt.
Office Address: Faculty
of Pharmacy, Beni-Suef University, Egypt.
Cellular Phone: +2 01286211181/
01060917535
E-mail Address: eglal_bardisi@yahoo.com.
University Website: www.bsu.edu.eg
Educational History
- Philosophy of Doctor (Ph.D) of Pharmaceutical
Sciences (Analytical Chemistry) Faculty of Pharmacy, Beni Suef University, February 2011.
- Master of Pharmaceutical Sciences (Analytical Chemistry)
Faculty of Pharmacy, Cairo University- Beni Suef Branch, September 2008.
- Bachelor of Pharmaceutical
sciences, Faculty of
Pharmacy,
Cairo University - Beni-Suef Branch, May 2003.
Occupational Background:
- Lecturer
in Analytical Chemistry, Faculty of Pharmacy, Beni-Suef University, Egypt. (2011-2015).
- Assistant
Lecturer in Analytical Chemistry Department, - Faculty of Pharmacy,
Beni-Suef University, Egypt. (2008-2011).
- Demonstrator
in Analytical Chemistry Department, Faculty of of Pharmacy, Beni-Suef
University, Egypt. (2004-2007).
Research Interest:
Pharmaceutical
Analytical Chemistry:
o
Chromatographic
methods (including HPLC, HPTLC and LC-MS).
o
Spectrophotometric
and spectrofluorimetric methods.
o
Multivariate
analysis.
o
Studying
drug stability in raw material and in their pharmaceutical preparations.
o
Analysis
of drugs in raw materials, pharmaceutical formulations and biological fluids,
whether in mixtures or in presence of metabolites, impurities or degradation
products.
Publications:
A- Pre-doctor publications
(4)
1-Simultaneous determination of methocarbamol and ibuprofen
or diclofenac potassium using mean centering of the ratio spectra method
Nouruddin W. Ali, Maha A. Hgazy, M Abdelkawy, Eglal A. Abdelaleem
Acta Pharmaceutica 62 (2), 191-200
2-Quantitative
determination of oxybutynin hydrochloride by spectrophotometry, chemometry and
HPTLC in presence of its degradation product and additives in different
pharmaceutical dosage forms
Nouruddin W. Ali, Maha A. Hgazy, M Abdelkawy, Eglal
A. Abdelaleem
Talanta 80 (5), 2007-2015
3-Simultaneous determination of
methocarbamol and its related substance (guaifenesin) in two ternary mixtures
with ibuprofen and diclofenac potassium by RP- HPLC method
Nouruddin W. Ali, Maha A. Hgazy, M Abdelkawy, Eglal A. Abdelaleem
Journal of Liquid Chromatography
& Related Technologies 35 (16), 2229-2242
4- Simultaneous Determination of
Methocarbamol and Its Related Substance (Guaifenesin) in Two Ternary Mixtures with Ibuprofen and Diclofenac
Potassium
Nouruddin W. Ali, Maha A. Hgazy, M Abdelkawy, Eglal A. Abdelaleem
Journal of Planar
Chromatography Modern TLC, 25 (2) (2012): 150-155.
B- Post-doctor publications
Publications
from master and doctor thesis (11)
1-Stability indicating spectrophotometric and
spectrodensitometric methods for determination of calcium dibesilate in the
presence of its impurity and / or degradation product
Nouruddin W. Ali, Maha A. Hgazy, Eglal A. Abdelaleem, M
Abdelkawy, Rehab M. Abdelfatah
International Journal of Pharmacy and Pharmaceutical
Sciences 5 (3) (2013)207-214
3-Linear Support Vector
Regression and Partial Least Squares Chemomertic Models for Determination of
Hydrochlorothiazide and Benazepril Hydrochloride in Presence of Related
Impurities: A Comparative Study
Ibrahim A. Naguib, Eglal A. Abdelaleema ,
Mohammed E. Draz and
Hala E. Zaazaa
Spectrochimica Acta Part A: Molecular and Biomolecular
Spectroscopy, 130 (2014) 350-356.
4-Two Validated Liquid Chromatographic
Methods for the Simultaneous Determination of Flumethasone Pivalate, Its
Related Substance (Flumethasone), and Clioquinol
Nouruddin W. Ali, Maha A. Hgazy, Eglal
A. Abdelaleem, M Abdelkawy, Rehab M. Abdelfatah
Journal of Planar Chromatography
Modern TLC, 27 (6) (2014): 466-471.
5-Simultaneous determination of
Hydrochlorothiazide and Benzapril Hydrochloride or Amiloride Hydrochloride
in presence of Hydrochlorothiazide impurities: Chlorothiazide and
Salamide by HPTLC method
Ibrahim
A. Naguib ,Eglal A. Abdelaleem, Hala E.
Zaazaa and Mohammed E. Draz
Journal
of chromatographic Science, 53 (2015) 183-188
6-Development and Validation of a
Stability-Indicating High-Performance Thin-Layer Chromatographic Method for
Determination of Pyridostigmine Bromide in the Presence of Its Alkaline-Induced
Degradation Product
Nouruddin W. Ali*,
Eglal A. Abdelaleem, Ibrahim A. Naguib, and Fatma
F. Abdallah
Journal of Planar Chromatography
Modern TLC, 28 (4) (2015): 316-322
7-Development and validation of
stability indicating spectrophotometric and HPTLC methods for determination of
acemetacin
Ibrahim A.
Naguib, Eglal A.
Abdelaleem, Hala E. Zaazaa, and Essraa A. Hussein
European
Journal of Chemistry 5 (2) (2014) 219-226
8-Spectrophotometric Methods for
Quantitative Determination of Binary Mixture of Hydrochlorothiazide and
Amiloride Hydrochloride without Prior Separation
Eglal A. Abdelaleem , Ibrahim A. Naguiba, Hala E. Zaazaa and
Mohammed E. Draz
Asian Journal of Biomedical
and Pharmaceutical Sciences,4(34) (2014)27-337-33
9-Development and Validation of RP-HPLC
Method for Determination of Hydrochlorothiazide, Amiloride Hydrochloride and
Related Impurities in Bulk and Pharmaceutical Dosage Forms
Ibrahim A. Naguib, Eglal A. Abdelaleem, Mohammed E. Draz,
Hala E. Zaazaa
Analytical Chemistry Letters 5 (2)2015 85 –
93
10- HPTLC and RP-HPLC methods for
simultaneous determination of Paracetamol and Pamabrom in presence of their
potential impurities
Eglal A. Abdelaleem, Ibrahim A. Naguib,
Eman S. Hassan,
Nouruddin W. Ali
Journal of Pharmaceutical and Biomedical Analysis 114 (2015) 22–27.
11-Novel
spectrophotometric determination of flumethasone pivalate and clioquinol in
their binary mixture and pharmaceutical formulation
Eglal
A. AbdelAleem, Maha A. Hegazy, Nouruddin W. Ali, M. Abdelkawy, Rehab M. Abdelfatah,
Spectrochimica Acta Part A: Molecular and Biomolecular
Spectroscopy, 136 (2015) 707-713.
12-Determination of Cefoperazone Sodium in
Presence of Related Impurities by Linear Support Vector Regression and Partial
Least Squares Chemometric Models
Ibrahim A. Naguib, Eglal A. Abdelaleem, Hala E. Zaazaa, and Essraa A. Hussein
Journal of Analytical Methods in Chemistry Volume 2015, Article ID
593892, 8 pages
2- Publications not from thesis (10)
1- Application of Fourier Function to Double
Divisor Ratio Spectra Curves for Analysis of Some Amoebicide Drugs in Their
Ternary Mixtures.
Nada S Abdelwahab and Eglal A Abdelaleem
PharmceuticaAnalyticaActa,, 3 (2) (2012).
2-
Validated stability indicating RP-HPLC method for determination of paracetamol,
methocarbamol and their related substances.
Eglal A. Abdelaleem and Nada S. Abdelwahab
Analytical Methods, 5 (2013) 241-245 DOI:10.1039/C2AY26085A
3-
Simultaneous determination of some antiprotozoal drugs in their binary and
ternary mixtures with mebeverine hydrochloride in different dosage forms.
Eglal
A. Abdelaleem and Nada S. Abdelwahab
Journal
of Liquid Chromatography and Related Technologies, 36: (2013) 1528–1539
4- TLC
Densitometric determination of guaifenesin, pseudoephedrine hydrochloride and
guaifenesine related substance (guaiacol).
Nada S.
Abdelwahab and Eglal A. Abdelaleem
Journal
of Planar Chromatography Modern TLC, 26 (1) (2013): 73-77.
5- Stability-Indicating
TLC–Densitometric Method for Simultaneous Determination of paracetamol and
Chlorzoxazone and their Toxic Impurities.
Eglal. A. Abdelaleem and Nada. S. Abdelwahab
Journal of Chromatographic Sciences 2012; 51(2): 187-191,
doi:10.1093/chromsci /bms125.
6-Validated chromatographic and
spectrophotometric methods for analysis of some amoebicide drugs in their
combined pharmaceutical preparation.
Eglal. A. Abdelaleem and
Nada. S. Abdelwahab
Pakistan journal of Pharmaceutical
Sciences, 26 (1) (2013)175-183.
7-
Simultaneous determination of some antiprotozoal drugs in different combined
dosage forms by mean centering of ratio spectra and multivariate calibration
with model updating methods.
Eglal. A. Abdelaleem and
Nada. S. Abdelwahab
Chemistry Central Journal
2012, 6:27
8-Mean
centering of ratio spectra and successive derivative ratio spectrophotometric
methods for determination of isopropamide iodide, trifluoperazine hydrochloride
and trifluoperazine oxidative degradate
Maha M.
Abdelrahman , Eglal A. Abdelaleem
"Journal of Saudi Chemical Society"2012
9- Stability Indicating RP-HPLC Method for
Simultaneous Determination of Guaifenesin and Pseudoephedrine Hydrochloride in
Presence of Syrup Excepients.
Nada. S.
Abdelwahab and Eglal. A. Abdelaleem
"Arabian Journal of Chemistry.",
accepted for publication November 2013
10-HPTLC Method for the Determination of
Paracetamol, Pseudoephedrine and Loratidine in Tablets and Human Plasma
Nehal
Fayek Farid ? , Eglal A.
Abdelaleem
accepted for publication in Journal of Chromatographic Sciences
Conferences Participation
1-Posters
presented at FUE International Conference on Pharmaceutical Technologies
(ICPT). Feb. 2012.
a- "Simultaneous determination
of some antiprotozoal drugs in different combined dosage forms by mean
centering of ratio spectra and multivariate calibration with model updating
methods"
Eglal A Abdelaleem,
Nada S Abdelwahab
2- Posters
presented in The 4th International Scientific Conference of Faculty
of Pharmacy, Cairo University, Entitled "Pharmacy Education and Community
Expectations". April 2013.
2a-Stability Indicating RP-HPLC Method for Simultaneous Determination of
Guaifenesin and Pseudoephedrine Hydrochloride in Presence of Syrup Excepients.
Nada.
S. Abdelwahab and Eglal. A. Abdelaleem.
2b- Stability
Indicating HPTLC Method for Determination of Ascorbic Acid, Paracetamol and
Guaifenesin in Their Ternary Mixture.
Maha. M. Abdelrahman, Nada. S. Abdelwahab and Eglal. A.
Abdelaleem.
2c-Development and Validation of Stability Indicating Spectrophotometric
and HPTLC Methods for Determination of Acemetacin
Ibrahim A. Naguib, Eglal A. Abdelaleem
, Hala E. Zaazaa and Essraa A. Hussein
3- Poster
presented in The 17th Scientific Congress of The Association of
Pharmacy Colleges in The Arab World" New Trends in Drug Discovery,
Development and Pharmacy Practice", Ein Shams University. October 2014.
"different
chromatographic methods for determination of carbazochrome and troxerutin in
pharmaceutical formulations".
Nouruddin W. Ali, , Maha. M. Abdelrahman, Eglal. A.
Abdelaleem,Raghda A.Emam
4-
Poster presented in 5th International Conference of pharmaceutical
and Drug Industries Research Division under the theme of Advances in
Pharmaceutical Research . March 2015
4a-"
simultaneous Determination of Theophylline, Guaifenesin and its Impurity
Guaicol by HPLC,TLC-spectrodensitometric Methods in Pure form and in Syrup
formulation
Eglal. A. Abdelaleem
, Ibrahim A.Naguib, Hala E.Zaazaa, shimaa A farag
4b-"
development of three spectrophotometric methods for determination of
pyridostigmine
Eglal. A. Abdelaleem,
Ibrahim A.Naguib, Fatma F.Abdallah ,Nouruddin W. Ali
4c-
HPTLC and RP-HPLC for determination of paracetamol and pamabrom
Nouruddin
W. Ali,
Ibrahim
A.Naguib, Eglal. A. Abdelaleem , Eman S.Hassan
5- Poster presented in The 1st International
Conference on Health between Nutrition and Treatment, Beni-Suef University
5a- "Development and
validation of three spectrophotometric Methods for simultaneous Determination
of Paracetamol and Pamabrom in Bulk and Pharmaceutical Formulation"
Eglal. A. Abdelaleem, Ibrahim A.Naguib, Eman
S.Hassan, Nouruddin W. Ali
,
5b-" Quantitative Determination of
Carbinoxamine Maleate and Pseudoephedrine HCl by Double Divisor-Ratio Spectra
Derivative Method and Multivariate Calibration With Model Updating in Presence
of Oral Drops Excipients"
Eglal. A. Abdelaleem,
Maha. M. Abdelrahman, Nouruddin W. Ali, Raghda A.Emam
General certificates:
o
International Computer driving
License (ICDL).
o
National TOEFL PBT (2009) score: 504.
Membership:
- Member in the Egyptian General Syndicate
of Pharmacists
- Member in Beni-Suef Syndicate of
Pharmacists.
Teaching
Experience:
o Teaching and supervising the practical courses of pharmaceutical
analytical Chemistry for the undergraduate students (first, second, fourth
& fifth year) in Faculty of Pharmacy, Beni-Suef University general and
clinical pharmacy programs.
o Oral examiner for undergraduate students in Faculty of pharmacy
Beni-Suef University and in other public and private universities.
o Teaching and supervising in pharmaceutical analytical Chemistry
for the postgraduate students in Faculty of Pharmacy, Beni-Suef University.
o Supervising many of master and Ph.D students (Pharmaceutical
analytical chemistry and Medicinal Chemistry).
o Working as academic advisor for clinical pharmacy program
students (since 2010).
o Supervising the summer training of undergraduate students at
Faculty of Pharmacy, Beni-Suef University.
Scientific Courses:
Under graduate students
- General and physical chemistry
- Qualitative analysis (analysis of
cations and anions)
- Volumetric analysis (acid base,
precipitmetry, complexometry, redox analysis)
- Chromatography courses (HPLC principles&
applications in pharmaceutical analysis).
- Instrumental analysis (principles and
applications of different instrumental techniques in pharmaceutical
analysis e.g. Spectroscopic methods (spectrophotometry,
Spectrofluorimetry, Atomic absorption…etc), chromatographic methods (HPLC,
GC, TLC…etc), electrochemical methods (conductometry, potentiometry…etc)).
- Quality control and quality assurance in
pharmaceutical industry.
- Electrochemical methods of analysis
(conductometry, potentiometry…etc).
Premaster courses:
1-
Advanced methods of instrumental
analysis (IR, MS and NMR spectrometry and spectrophotometry).
2-
Quality control in pharmaceutical
industry.
3-
Separation analysis techniques
(GC, TLC, HPLC, UPLC, LC-MS and Electrophoresis).
4-
Stability indicating methods of
analysis.
Master Title
Analytical Study on Some Drugs Used in Ear and Eye Drops
Master Abstract
ABSTRACT
This thesis is concerned with analytical study of some drugs used in ear and eye drops, representing different chemical classes. namely Phenylephrine HCl , Cyclopentolate HCl , Ciprofloxacin HCl , Hydrocortisone , Chloramphenicol , Dexamethasone Sodium Phosphate , Tetrahydrozoline HCl (TETRA), Clioquinol , Flumethasone Pivalate .
The aim of this work is to develop simple, rapid, sensitive and selective methods for simultaneous determination of the cited drugs in their mixtures in pure forms or in pharmaceutical preparations.
The thesis comprises four parts:
PART 1 :
Simultaneous Determination of Phenylephrine HCl and Cyclopentolate HCl in Pure Forms and in Pharmaceutical Preparation.
This part comprises four sections:
Section (A) : Simultaneous Determination of Phenylephrine HCl and Cyclopentolate HCl by Spectrophotometric Method.
In this section, Phenylephrine HCl could be determined in presence of Cyclopentolate HCl using a zero order spectrum with an analytical useful maximum at ?max 275 nm. The absorbance obeyed Beer's law over concentration range 4 - 40µg.mL-1 with mean percentage recovery 99.77± 1.092.While determination of Cyclopentolate HCl in presence of Phenylephrine HCl was obtained by third derivative D3 spectrophotometry at ?max222.2 nm. The peak height response obeyed Beer's law over concentration range 1–10 µg.mL-1 with mean percentage recovery 99.86 ± 1.379.
Section (B): Simultaneous Determination of Phenylephrine HCl and Cyclopentolate HCl by Spectrodensitometric Method.
In this section, both drugs are separated on a silica gel plate using ethylacetate : methanol : ammonia solution(48 : 12: 2.4 by volume) as mobile phase and UV detection of Phenylephrine HCl band at 254 nm over a concentration range of 1- 9µg.band -1 with mean percentage recovery of 100.31±1.293 and Cyclopentolate HCl band was detected at ?max 210 nm over a concentration range of 2 - 8µg.band -1 with mean percentage recovery of 100.56± 1.251 .
Section (C): Determination of Cyclopentolate HCl by The Colorimetric Method (Ternary Complex) in Presence of Phenylephrine HCl.
This section includes a colorimetric determination of Cyclopentolate HCl in presence of Phenylephrine HCl through formation of ternary complex. A bluish green color was obtained which can be measured at ?max 625 nm.
The absorbance obeyed Beer's law over concentration range 10 - 70 µg.mL -1 with mean percentage recovery 100.69± 0.720. The selectivity of the proposed method was checked using laboratory prepared mixtures and it was successfully applied to the analysis of the pharmaceutical preparation containing Cyclopentolate HCl with no interference from Phenylephrine HCl and other dosage form additives .
Section (D): Determination of Phenylephrine HCl by The Colorimetric Method (Diazotization Coupling Technique) in Presence of Cyclopentolate HCl.
This section includes a colorimetric determination of Phenylephrine HCl in presence of Cyclopentolate HCl using diazotization coupling technique method. Yellow color was obtained which can be measured at ?max 460 nm. The absorbance obeyed Beer's law over concentration range 4 - 10 µg.mL -1 with mean percentage recovery 100.02±0.488.
PART ll :
Simultaneous Determination of Ciprofloxacin HCl and Hydrocortisone in Pure Form and in Pharmaceutical Preparation.
This part comprises four sections:
Section (A): Simultaneous Determination of Ciprofloxacin HCl and Hydrocortisone by Spectrophotometric Method.
In this section, Ciprofloxacin HCl could be determined in presence of Hydrocortisone using a zero order spectrum with an analytical useful maximum at ?max 322 nm. The absorbance obeyed Beer's law over concentration range 1 - 12 µg.mL-1 with mean percentage recovery 99.63 ± 1.352. Determination of Hydrocortisone in presence of Ciprofloxacin HCl was obtained by simultaneous use of the first derivative of the ratio spectra (1DD) with measurements at 255.8 nm using the spectrum of 12µg.mL -1of Ciprofloxacin HCl as a divisor over a concentration range of 1–25µg.mL-1 with mean percentage recovery 100.11 ± 0.833.
Section (B): Simultaneous Determination of Ciprofloxacin HCl and Hydrocortisone by The Spectrodensitometric Method.
In this section, both drugs are separated on a silica gel plate using chloroform : methanol : benzene : ammonia solution (57: 21 : 25.5: 3 by volume ) as mobile phase and UV detection of Ciprofloxacin HCl band at 254 nm over a concentration range of 0.2 - 1 µg.band -1with mean percentage recovery of 99.62 ± 0.421. Hydrocortisone band was detected at 245nm over a concentration range of 0.3 – 1.4 µg.band -1 with mean percentage recovery of 99.8 ± 1.291.
Section (C): Multivariate Spectrophotometric Technique for Determination of Ciprofloxacin HCl and Hydrocortisone Mixture.
Two chemometric techniques, Principle component regression (PCR ) and Partial least squares ( PLS ) have been successfully applied for simultaneous determination of Ciprofloxacin HCl and Hydrocortisone in pure forms and in pharmaceutical preparation .CLS has been applied for pure forms only .Training set of 10 mixtures containing different ratios of Ciprofloxacin HCl and Hydrocortisone is used for construction of the three models .
Section (D): Determination of Ciprofloxacine HCl in presence of Hydrocortisone by the Spectrofluorimetric Method.
This section includes studying different factors affecting the native fluorescence of Ciprofloxacin HCl including the solvents, different surface active agent, different pH values and different excitation and emission wavelengths. Also the stability of Ciprofloxacin HCl fluorescence intensity by time is studied.
PART lll:
Simultaneous Determination of Chloramphenicol, Dexamethasone Sodium Phosphate and Tetrahydrozoline HCl by The Spectrophotometric Method in Their Ternary Mixtures and Multivariate Spectrophotometric Method in Their Ternary Mixtures and in Presence of Chloramphenicol Degradate .
This part comprises three sections:
Section (A): Simultaneous Determination of Chloramphenicol, Dexamethasone Sodium Phosphate and Tetrahydrozoline HCl by Spectrophotometric Method in Their Ternary Mixtures.
In this section, the first derivative D1 spectrophotometric method is applied for determination of Chloramphenicol in presence of Tetrahydrozoline HCl and Dexamethasone Sodium Phosphate at ?max 295 nm in the range of 5 – 60µg.mL -1 with mean percentage recovery of 99.74 ± 1.816 .
Dexamethasone Sodium Phosphate was determined by simultaneous use of the first derivative of the ratio spectra ( 1DD) with measurements at ?max 262.4 nm using the spectrum of 6µg.mL -1of Tetrahydrozoline HCl as a divisor over a concentration range of 5 – 25µg.mL-1with mean percentage recovery 99.82 ± 1.631.
Tetrahydrozoline HCl was determined by simultaneous use of the first derivative of the ratio spectra (1DD) with measurements at ?max236.6nm using the spectrum of 60µg.mL -1of Chloramphenicol as a divisor over a concentration range of 3 – 18 µg.mL-1with mean percentage recovery100.73 ± 0.765 .
Section (B): Simultaneous Determination Chloramphenicol, Dexamethasone Sodium Phosphate and Tetrahydrozoline HCl by The Multivariate Spectrophotometric method in Their Ternary Mixtures.
Two chemometric techniques, Principle component regression (PCR ) and Partial least squares (PLS) have been successfully applied for simultaneous determination of Chloramphenicol, Dexamethasone and Tetrahydrozoline HCl in pure forms and in pharmaceutical preparations .Training set of 13 mixture containing different ratios of Chloramphenicol, Dexamethasone and Tetrahydrozoline HCl is used for construction of the two models .
Section (C): Simultaneous Determination of Chloramphenicol, Dexamethasone Sodium Phosphate and Tetrahydrozoline HCl by The Multivariate Spectrophotometric method in Presence of Chloramphenicol Degradate .
Two chemometric techniques, Principle component regression (PCR) and Partial least squares ( PLS ) have been successfully applied for simultaneous determination of Chloramphenicol, Dexamethasone Sodium Phosphate and Tetrahydrozoline HCl and Chloramphenicol Degradate in pure forms and in pharmaceutical preparations. Training set of 16 mixture containing different ratios of Tetrahydrozoline HCl , Dexamethasone and Chloramphenicol is used for construction of the two models.
PART lV:
Simultaneous Determination of Clioquinol and Flumethasone Pivalate in Pure Forms and in Pharmaceutical Preparations .
This part comprises two sections:
Section (A): Simultaneous Determination of Clioquinol and Flumethasone Pivalate by Spectrophotometric Method.
In this section, Clioquinol could be determined in presence of Flumethasone Pivalate using a zero order spectrum with an analytical useful maximum at 328nm. The absorbance obeyed Beer's law over concentration range 1 - 9 µg.mL -1 with mean percentage recovery 99.99 ±0.875. Determination of Flumethasone pivalate in presence of Clioquinol was obtained by simultaneous use of the first derivative of the ratio spectra (1DD) with measurements at ?max 241 nm using the spectrum of 50µg.mL -1of Clioquinol as a divisor over a concentration range of 1–20µg.mL-1 with mean percentage recovery 100.68 ± 1.193.
Section (B): Simultaneous Determination of Clioquinol and Flumethasone Pivalate by The Spectrodensitometric Method.
In this section, both drugs are separated on a silica gel plate using ethylacetate : hexane : benzene : 96 % acetic acid ( 35 : 21 : 5 : 0.35 by volume) as mobile phase and UV detection of both bands at 254 nm . Clioquinol was determined over a concentration range of 0.6 – 2.2 µg.band -1 with mean percentage recovery of 99.92 ± 0.983 while Flumethasone Pivalate was determined over a concentration range of 0.3 – 1.6 µg.band -1 with mean percentage recovery of 99.85 ± 1.914.
PHD Title
Analytical and Stability Studies of Some Nitrogenous Compounds of Different Pharmacological Activities
PHD Abstract
This thesis consists of five parts in addition to references and an Arabic summary. Each part includes an introduction, literature review, descriptive experimental work for the studied drugs, results, discussion and ends with a conclusion.
Part I: Quantitative Determination of Oxybutynin Hydrochloride in Presence of Its Degradation Product and Additives in Different Pharmaceutical Dosage Forms
This part includes five sections.
Section (A): Introduction and Literature Review
This section includes literature review about chemical structure, physical properties and pharmacology of Oxybutynin Hydrochloride (OX), it also includes review of methods of analysis developed for determination of OX either alone or in presence of its degradation product in pure form and in pharmaceutical formulations.
Section (B): Determination of Oxybutynin Hydrochloride in Presence of Its Degradation Product by First Derivative of Ratio Spectra Method (1DD)
In this section the first derivative of ratio spectra spectrophotometric technique (1DD) has been applied to improve selectivity for determination of OX in presence of its degradation product (OX Deg) using 0.1N HCl as a solvent. OX was determined by dividing the absorption spectra of different concentrations of OX in the range of 6 - 28 µg.mL-1 by the absorption spectrum of 20µg.mL-1 of its degradation product. The obtained ratio spectra were differentiated with respect to wavelength and the 1DD values at 216 nm were recorded. The proposed method was successfully applied for determination of OX in Uripan® and Detronin® tablets. The results obtained by applying the proposed method were statistically compared to those obtained by applying a reported HPLC method and no significant difference were found regarding both accuracy and precision.
Section (C): Determination of Oxybutynin Hydrochloride in Presence of its Degradation Product by Mean Centering of Ratio Spectra Method
A recent and simple method was developed for determination of OX in presence of its degradation product. In this method OX was determined by measuring the amplitudes of the mean centered ratio spectra at 217.8 nm using 20 µg.mL-1 of its degradation product as a divisor. The proposed method was used for determination of OX in tablets and the results of standard addition technique confirmed that tablet additives did not interfere.
Section (D): Determination of Oxybutynin Hydrochloride in Presence of its Degradation Product and Additives in Different Pharmaceutical Formulations by Multivariate Calibration Methods
Multivariate calibrations models, such as PCR and PLS have been successfully applied as selective stability indicating methods for determination of OX in presence of its degradation product. The two chemometric PCR and PLS methods were successfully applied for the determination of OX in Uripan® and Detronin ® tablets.
In order to apply the developed methods for determination of OX in Uripan ® syrup and Detronin ® syrup, model updating was performed.
To validate the predictive ability of the developed models, they were applied to predict the concentrations of OX and its degradation product in an external validation set. Statistical analysis of the results obtained by the developed models were compared with a reported HPLC one, indicating no significant difference regarding both accuracy and precision.
Section (E): Determination of Oxybutynin Hydrochloride in Presence of Its Degradation Product and Additives in Different Pharmaceutical Formulations by HPTLC-Densitometric Method
In this section HPTLC-Densitometric method was developed by separating OX from its degradation product, methylparaben and propylparaben successfully and efficiently using chloroform: methanol: ammonia solution: triethylamine (100: 3: 0.5: 0.2 by volume) as a mobile phase. The separated bands of OX were scanned at 220 nm in the range of 2–14 µg.band-1. The proposed HPTLC-Densitometric method was applied successfully for determination of OX in different pharmaceutical formulations.
Part II: Stability Indicating Methods for Determination of Flavoxate Hydrochloride in Presence of Its Alkaline Induced Degradation Products
This part includes six sections.
Section (A): introduction and literature Review
This section includes literature review about chemical structure, physical properties and pharmacology of Flavoxate Hydrochloride (FL), it also includes review of methods of analysis developed for determination of FL either alone or in presence of its degradation product in pure form and in pharmaceutical formulations.
Section ( B): Determination of Flavoxate Hydrochloride in Presence of Its Alkaline Induced Degradation Products by First Derivative Spectrophotometry (1D)
In this section, a first derivative spectrophotometric method was developed for determination of FL in methanol at 275 and 331 nm. Good linearity was obtained in the range of 2- 16 µg.mL-1. The proposed method retained its accuracy in presence of up to 80 % of FL alkaline induced degradation products (FL Degs). The proposed method has been applied for determination of FL in its pharmaceutical formulations.
Section ( C ): Determination of Flavoxate Hydrochloride in Presence of Its Alkaline Induced Degradation Products by First Derivative of Ratio Spectra method (1DD)
In this section the first derivative of ratio spectra amplitudes at 268 nm and 291 nm were used for determination of FL in presence of its alkaline induced degradation products in the range of 2 - 16 µg.mL-1. The suggested method was successfully applied for determination of FL in its pharmaceutical formulation.
Section ( D ): Determination of Flavoxate Hydrochloride in Presence of its Alkaline Induced Degradation Products by Multivariate Calibration Models.
In this section two chemometric models PCR and PLS were used for simultaneous determination of FL and its alkaline induced degradation products .Training set of 14 mixtures containing different ratios of FL and its alkaline induced degradation products was used for construction of the two models.. Satisfactory results were obtained on applying the proposed methods for the analysis of FL in its pharmaceutical formulation.
Section ( E): Determination of Flavoxate Hydrochloride in Presence of its Alkaline Induced Degradation Products by TLC-Densitometry
In this section, TLC-Densitometric method was developed by separating FL from its alkaline induced degradation products using chloroform: methanol: glacial acetic acid (90: 6: 3 by volume) as a mobile phase. The proposed TLC-Densitometric method was applied successfully for determination of FL in its pharmaceutical formulation.
Section ( F: Determination of Flavoxate Hydrochloride in Presence of Its Alkaline Induced Degradation Products by RP-HPLC Method
In this section, an accurate and selective RP-HPLC method has been investigated and validated for quantitative analysis of FL in presence of its alkaline induced degradation products. The chromatographic separation was achieved using methanol: acetonitrile: deionized water: triethylamine (100: 50: 36: 1, by volume; pH was adjusted to 6.5 with orthophosphoric acid) as a mobile phase, the flow rate was 2 mL.min-1 with UV detection at 254 nm.
The proposed method was validated and applied for determination of FL in its pharmaceutical formulation. When results obtained by applying the proposed method for analysis of FL were compared to those obtained by applying a reported HPLC method, no significance difference was observed.
Part III: Determination of Methocarbamol and Ibuprofen in Their Binary Mixture and in Presence of Methocarbamol Degradation Product
This part comprises five sections
Section (A) : introduction and literature Review
This section includes literature review about chemical structure, physical properties and pharmacology of Methocarbamol (ME) and Ibuprofen (IB), it also includes review of methods of analysis developed for determination in their single formulation and in their binary mixture.
Section (B): Simultaneous Determination of Methocarbamol and Ibuprofen by First (1D) and Second (2D) Derivative Spectrophotometry
This section includes two spectrophotometric methods for simultaneous determination of Methocarbamol and Ibuprofen in their binary mixture. The developed spectrophotometric methods include first and second derivative methods. The first derivative amplitudes at 283 nm were used for determination of ME concentrations, while second derivative amplitudes at 231.6 nm were used for determination of Ibuprofen.
Section (C): Simultaneous Determination of Methocarbamol and Ibuprofen by Mean Centering of Ratio Spectra Method.
A recent and simple method was developed for simultaneous determination of ME and IB in their binary mixture, without prior separation steps.
In this method, the mean centered ratio spectra amplitudes at 218.4 nm were used for determination of ME and IB. Moreover the suggested method has been applied for determination of the cited drugs in their commercial tablets.
Section (D): Simultaneous Determination of Methocarbamol and Ibuprofen by TLC- Densitometry in Presence of Methocarbamol Degradation Product.
In this section TLC-Densitometric method was developed by separating ME and IB in presence of Methocarbamol degradation product successfully and efficiently using ethylacetate: acetone: formic acid: triethylamine (62: 35: 0.3: 6 by volume) as a developing system. The separated bands of ME and IB were scanned at 278 nm and 222 nm for ME and IB respectively
The suggested method is applicable for determination of both drugs in its pharmaceutical formulation.
Section (E): Simultaneous Determination of Methocarbamol and Ibuprofen by RP- HPLC method in Presence of Methocarbamol Degradation Product.
In this section, an accurate and selective RP-HPLC method has been investigated and validated for quantitative analysis of ME and IB in presence of Methocarbamol degradation product. In this method, an isocratic elution of the three components was performed at ambient temperature on C18 column with a mobile phase consisting of 0.05 M KH2PO4 (pH = 7): acetonitrile: methanol (90: 25: 15 by volume), using flow rate 1.2 mL.min-1 and UV detection at 220 nm.
By applying the suggested RP-HPLC method, ME and IB could be quantified in the range of 6 – 20 and 6 – 28 µg.mL-1 for ME and IB, respectively.
Statistical comparison of the results obtained by the proposed method and a reported HPLC one for analysis of pure ME and IB was carried out. The values of the calculated t and F are less than the tabulated ones which reveals that there is no significant difference between the two methods with respect to accuracy and precision.
Part IV: Determination of Methocarbamol and Diclofenac Potassium in Their Binary Mixture and in Presence of Methocarbamol Degradation Product
This part comprises six sections
Section (A) : introduction and literature Review
This section includes literature review about chemical structure, physical properties and pharmacology of Methocarbamol (ME) and Diclofenac Potassium (DI) it also includes review of methods of analysis developed for determination in their single formulation and in their binary mixture.
Section (B): Simultaneous Determination of Methocarbamol and Diclofenac potassium by First (1D) and Second Derivative Spectrophotometry (2D)
In this section, derivative spectrophotometric technique was used , for determination of Methocarbamol and Diclofenac Potassium in their binary mixture. Methocarbamol was determined by measuring peak amplitude at 225.4 nm for 2D method while Diclofenac Potassium can be determined at 297 nm using 1D method using 0.1 N HCl as blank. Satisfactory results were obtained on applying the proposed methods for the analysis of the two mentioned drugs in their commercial tablets, the results obtained were statistically compared with that obtained by the reported HPLC method indicating no significant difference between them.
Section (C): Simultaneous Determination of Methocarbamol and Diclofenac Potassium by Mean Centering of Ratio Spectra Method
A simple spectrophotometric method has been investigated for simultaneous determination of both Methocarbamol and Diclofenac Potassium without prior separation steps. in this method , ME was determined by measuring the amplitudes of the mean centered ratio spectra at 279.4 nm and 260.6 nm using 6 µg.mL-1 of DI as a divisor. While DI was determined by measuring the amplitudes of the mean centered ratio spectra at 260.8 nm. The proposed method was used for quantitation of both ME and DI in Dimra ® tablets where satisfactory results were obtained and its validity was further assessed by applying the standard addition technique.
Section (D): Simultaneous Determination of Methocarbamol and Diclofenac Potassium by Chemometric Method in Presence of Methocarbamol Degradation Product and Application of Model Updating for Determination Methocarbamol and Ibuprofen in Ibuflex® Tablets
In this section PLS model has been successfully applied as selective stability indicating method for determination of the ternary mixture of ME, DI and Methocarbamol degradation product.
To validate the predictive ability of the developed model it was applied to predict the concentrations of ME, DI and Methocarbamol degradation product in an external validation set.
In order to apply the developed method for determination of ME and IB in Ibuflex® tablets model updating was performed.
The investigated chemometric method was successfully applied for quantitation of the above mentioned drugs in Dimra® and Ibuflex® tablets with good percentage recoveries and good agreement with the labeled amounts. The results obtained by applying the developed model showed no significant difference when compared to those obtained by applying a reported HPLC.
Section (E): Simultaneous Determination of Methocarbamol and Diclofenac potassium by TLC- Densitometry in Presence of Methocarbamol Degradation Product
In this section TLC-Densitometric method was developed by separating ME and DI in presence of Methocarbamol degradation product successfully and efficiently using ethylacetate: acetone: formic acid: triethylamine (62: 35: 0.3: 6 by volume) as a developing system. The separated bands of ME and DI were scanned at 278 nm
The suggested method is applicable for determination of both drugs in their pharmaceutical formulation.
Linear relationships were obtained between the integrated peak area ×10-4 and the corresponding concentrations in the concentration range of 2 - 12 µg.band-1 for ME and 0.2 - 2.2 µg.band-1 for DI.
Section (F): Simultaneous Determination of Methocarbamol and Diclofenac Potassium by RP- HPLC Method in Presence of Methocarbamol Degradation Product.
A precise, specific, accurate and stability indicating RP- HPLC method was proposed for the determination of ME and DI in presence of Methocarbamol degradation product. In this method, an isocratic elution of the three components was performed at ambient temperature on C18 column with a mobile phase consisting of 0.05 M KH2PO4 (pH = 7): acetonitrile (80: 30 v/v), using flow rate of 1.45 mL.min-1 and UV detection at 278 nm.
The suggested method has been applied for determination of the two proposed components in commercial tablets. When results obtained by applying the proposed method for analysis of pure ME and DI were compared to those obtained by applying a reported HPLC method, no significant difference was observed.
Part V: Appendix
This part includes a brief idea about the instruments, solvents and chemicals used in other parts. In addition, detailed preparation of the standard solutions used in each part through this work was described in addition to method of preparation of Oxybutynin and Flavoxate degradation products.