نسرين
نسرين

Nessreen Salah Eldin Abdelhamid

lecturer

Basic Informations

C.V

Curriculum Vitae

Name:                              Nessreen Salah Eldin Abdelhamid Mohamed                                                                                                                

Position:                          Lecturer of Pharmaceutical analytical chemistry                         

Nationality:                     Egyptian.                                                                         

Date of Birth:                  March 5, 1980.

Address:                          1) 8a Fatema Alzahraa street, Beni-Suef, Egypt.

2) Faculty of Pharmacy, Beni-Suef University, El Shahid Ahmed Hegazi Street, Beni-Suef, 62514, Egypt

Mobile:                            +2 01144010107.

E-mails:                          1 - nesserinsalah@gmail.com

                                       2- nesreen.abdelhameed@pharm.bsu.edu.eg  

Degrees:                            

1)      B.Sc. of Pharmaceutical sciences (Excellent with honor degree), Cairo University, Beni-Sueif Branch, 2002.

2)     M.Sc. Pharmaceutical Analytical Chemistry, Cairo University, 2009.

3)     Ph.D. Pharmaceutical Analytical Chemistry, Beni-Suef University, 2014.

Experiences:

1-    Demonstrator of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Beni-Suef University, 30/12/2002.

2-    Assistant lecturer of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Beni-Suef University, 8/2/2010.

3-    Lecturer of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Beni-Suef University, 24/12/2013 and till now.

Noticing that:

1- The research unit at Beni-Suef branch of Cairo University was completed at July 2002.

2- Beni-Suef University, Egypt (was separated from Cairo University according to the Republic role No [192/2005] starting 1 August 2005).

3-        All courses and exams (written, oral, and practical) during undergraduate and graduate studies were in English.

Fields of research and routine work:

Research in analytical methods for drugs and related substances in bulk forms and pharmaceutical formulations including; spectrophotometry, HPLC, HPTLC, GC and chemometrics.

Brief description of duties:                                                                                                            

  • · Teaching of Analytical Chemistry-1 for undergraduate students of Program of pharmaceutical Sciences and Program of Clinical Pharmacy.
  • · Teaching of Analytical Chemistry -2 for undergraduate students of Program of pharmaceutical Sciences and Program of Clinical Pharmacy .
  • · Teaching of Analytical Chemistry -3 for undergraduate students of Program of pharmaceutical Sciences.
  • · Teaching of Instrumental Analysis for undergraduate students of Program of pharmaceutical Sciences and Program of Clinical Pharmacy.
  • · Teaching of Drug quality Control And Analysis for undergraduate students of Program of Clinical Pharmacy.                                                                                                                          
  • · Teaching of postgraduate students special courses of Advanced Methods Of Analysis,   Thermal Analysis,  and Functional Group Analysis.
  • · Supervision on the practical sections of undergraduates.
  • · Participating in preparation of final written and practical exams  as well as periodic exams of undergraduates.  
  • · Supervision on master and Ph.D. Theses of Postgraduates.

Activities:

1) Coordinator of post-graduate studies standard committee in the Quality Assurance Unit (QAU) in Faculty of Pharmacy , Beni-Suef University (10/2016 till now).

2) Member of the internal audit committees in the Quality Assurance Unit (QAU) in the academic years 2017/2018 – 2018/2019.

3) Pharmaceutical analytical chemistry department board honest and member (October 2017 – September 2019).

4) Member of the Faculty board since January 2020.

5) Member of “Beni Suef National University, Faculty of pharmacy regulation statute establishment committee” since 17th Sept.2020.

6) Member of the Egyptian Pharmacists Syndicate.

Attendance of Symposia

1) Attendance of the symposium entitled “Good Researcher And International Publishing” held in Beni-Suef University, Sept. 18th, 2016.

2) Attendance of the symposium entitled “How to prepare proposals of research projects, writing and financing steps” held in Beni-Suef University, Oct. 4th, 2016.

3) Attendance of the symposium entitled “Spreading the culture of QUALITY ” held by the Quality Assurance Unit (QAU) in Faculty of Pharmacy , Beni-Suef University. Part 1 (Oct. 21, 2018) & part 2 (Oct. 30, 2018).

4) Attendance of the symposium entitled “Industrial safety ” held by the Quality Assurance Unit (QAU) in Faculty of Pharmacy , Beni-Suef University. Feb. 17th, 2019.

5) Attendance of the symposium entitled “Awareness of the ministerial modifications to the faculty regulation statute ” held by the Quality Assurance Unit (QAU) in Faculty of Pharmacy , Beni-Suef University. Feb. 24th, 2019.

Professional workshops

1) Attendance of the workshop entitled “LC-MS-MS Basics and Applications” held by the Quality Assurance Unit (QAU) in Faculty of Pharmacy , Beni-Suef University. Sept. 13th , 2018.

2) Attendance of the workshop entitled “Separation And Flash Chromatography Solutions” held in the Faculty of Pharmacy , Fayoum University. Sept. 18th , 2018.

3) Attendance of the workshop entitled “Liquid Chromatography Mass Spectrometry LC-MS Basics and Applications” held by  Nawah Scientific centre. July. 11-15 , 2020.

4) Attendance of the course entitled “Biostatistics : Basics and Applications” held by  Nawah Scientific centre. August. 22-24 , 2020.

5) Attendance of the course entitled “Gas Chromatography Mass Spectrometry GC-MS Basics and Applications” held by  Nawah Scientific centre. Sept.. 27-29 , 2020.

Scientific siminars

1) Attendance of the seminar entitled “Green Chemistry And Green Analytical Chemistry” held by the Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy , Beni-Suef University. Feb. 27th , 2018.

2) Attendance of the seminar entitled “Experimental Design” held by the Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy , Beni-Suef University. March. 27th , 2018.

3) Attendance of the seminar entitled “ICH Guidelines, Highlights On Analytical Method Validation” held by the Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy , Beni-Suef University. April. 24th , 2018.

4) Attendance of the seminar entitled “Ion Selective Electrode” held by the Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy , Beni-Suef University. July. 31st, 2018.

5) Attendance of the seminar entitled “Gas Chromatography , Tips And Precautions” held by the Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy , Beni-Suef University. Oct. 30th , 2018.

Training workshops from “Human Resource Development Centre” Beni-Suef University:

1) The training workshop entitled “Research Team Management” Dec. 30th & 31st  , 2018.

2) The training workshop entitled “Student Evaluation and Examination Techniques” March. 3rd  & 4th  , 2020.

3) The training workshop entitled “Integrity, Transparency and Anti-corruption” May. 5th & 6th  , 2020.

4) The training workshop entitled “Use of Technology in Teaching” June. 14th &15st  , 2020.

5) The training workshop entitled “Time And Meeting Management” June. 17th & 18st, 2020.

6) The training workshop entitled “Effective Presentation Skills” held in the Center of Human Resources Development , Beni-Suef University. June. 21st & 22nd, 2020.

Other courses and workshops:

1) Attendance of the workshop entitled “Use And Activation Of EKB Gate” held by digital library project in Beni-Suef University, March. 8th & 9th , 2017.

2) Attendance of the workshop entitled “Updating of course specifications” held by the Quality Assurance Unit (QAU) in Faculty of Pharmacy , Beni-Suef University. Part 1 (Oct. 31, 2017) & part 2 (Nov. 7th & 8th, 2017)  .

3) Attendance of the workshop entitled “Postgraduate course specifications” held by the Quality Assurance Unit (QAU) in Faculty of Pharmacy , Beni-Suef University. Nov. 28th , 2017.

4) Attendance of the workshop entitled “Exams and control affairs” held by the Quality Assurance Unit (QAU) in Faculty of Pharmacy , Beni-Suef University. Nov. 29th , 2017.

5) Attendance of the workshop entitled “Modern teaching methods” held by the Quality Assurance Unit (QAU) in Faculty of Pharmacy , Beni-Suef University. Feb. 26th, 2019.

6) Attendance of the workshop entitled “First aid and rescue methods in emergency cases” held by the Quality Assurance Unit (QAU) in Faculty of Pharmacy , Beni-Suef University. March. 3rd , 2019.

7) Attendance of the workshop entitled “Scenario of buildings evacuation” held by the Quality Assurance Unit (QAU) in Faculty of Pharmacy , Beni-Suef University. March. 26th , 2019.

8) Participation in the module entitled “University Exams And Digital Question Banks” held by the DAAD Kairo Akademie at the premises of Beni-Suef University. Dec. 18th , 2019.

Scientific conferences:

1) Participation  by a poster in  “2nd International Conference of Faculty of Pharmacy, Ain Shams University – 2nd ICPASU” 13 – 15th Nov.  2018.

2) Participation  by a poster in  “5th FUE International Conference of Pharmaceutical Sciences” held by Future University ,28 – 30th  Jan.  2019.

3) Participation  by a poster in  “NUB 2nd Conference of Scientific Research in Pharmacy” held in Faculty of Pharmacy , Nahda University. 11 – 12th March,  2019.

4) Participation  by a poster in  “The 2nd Pharmaceutical Scientific Conference” held in Faculty of Pharmacy , Beni-Suef University. April. 4th , 2019.

Thesis:

Nessreen Salah Eldin Abdelhamid, (2009). Analytical Study of Some Drugs Affecting Respiratory System. Thesis for M.Sc. degree. Faculty of Pharmacy, Beni-Suef University.  

Nessreen Salah Eldin Abdelhamid, (2013). Analytical Study of Some Pharmaceutical Compounds Acting On The Respiratory System. Thesis for Ph.D. degree. Faculty of Pharmacy, Beni-Suef University.

Computer skills:

ICDL equivalent certificate, Supreme Council of Universities, CUICTT, Egypt, January 20, 2007.

Publications:

1-Fadia H. Metwally, M. Abdelkawy and Nessreen S. Abdelhamid. Application of spectrophotometric and GC techniques for simultaneous determination of diphenhydramine hydrochloride and menthol in pharmaceutical preparations. The Bulletin Of Faculty Of Pharmacy Cairo University. 2009; 47:1-15.

2- Fadia H. Metwally, M. Abdelkawy and Nessreen S. Abdelhamid. Application of spectrophotometric and thin layer chromatographic techniques for simultaneous determination of ambroxol hydrochloride and doxycycline hyclate in pharmaceutical preparations. The Bulletin Of Faculty Of Pharmacy Cairo University. 2009; 47:17-34.

3- Nouruddin W. Ali , M. Abdelkawy  and Nessreen S. Abdelhamid. Simultaneous determination of paracetamol and diphenhydramine hydrochloride mixture in the presence of their degradation products. International organization of scientific research (IOSR), Journal of Pharmacy and        Biological Sciences.2013;6(5):44-52.

 

4- Nouruddin W. Ali , M. Abdelkawy  and Nessreen S. Abdelhamid. Determination of oxeladin citrate in the presence of two of its degradationproducts by HPTLC and HPLC. International Journal of Pharmacy and Pharmaceutical Sciences.2013;5(4) ; 282-289.

5- Amal Khorshid, Nessreen S. Abdelhamid, Eglal A. Abdelaleem and Mahmoud M. Amin. Simultaneous determination of metformin and pioglitazone in presence of metformin impurity by different spectrophotometric and TLC – densitometric methods. SOJ Pharmacy & Pharmaceutical Sciences. 2018; 5(3) : 1–8.

6-  Eglal A. Abdelaleem, and Nessreen S. Abdelhamid. An innovative method, interference subtraction, for determination of drugs in syrups in presence of potential interfering excipients. Analytical Chemistry Letters. 2018; 8 (6) : 782 – 793.

 

7- Nessreen S. Abdelhamid , Eglal A. Abdelaleem, Amal Khorshid and Mahmoud M. Amin. Determination of antihypertensive drugs by using ratio difference spectrophotometric method. European journal of chemistry. 2019;10(1): 12-18.

8- Nessreen S. Abdelhamid , Mohammed T. Elsaady , Nouruddin W. Ali and  Walaa G. Abuelazem. Simultaneous determination of repaglinide, metformin hydrochloride and melamine by new HPLC and HPTLC chromatographic methods.  Analytical Chemistry Letters. 2019; 9(3): 418 – 429.

9- Maimana A. Magdy, Basma H. Anwar, Ibrahim A. Naguib and Nessreen S. Abdelhamid. Quantitative determination of Dapoxetine hydrochloride and Tadalafil using different validated spectrophotometric methods. Spectrochimica Acta Part A. 2019; 226: 117611.

10- Basma H. Anwar, Nessreen S. Abdelhamid, Maimana A. Magdy and Ibrahim A. Naguib. A Comparative Chemometric Study for Quantitative Determination of
Duloxetine Hydrochloride in the Presence of its Toxic Impurity 1-Naphthol. Current Pharmaceutical Analysis. 2019; 15:00-00.

11- Ibrahim A. Naguib, Maimana A. Magdy, Basma H. Anwar and Nessreen S. Abdelhamid . A Validated Green HPTLC Method for Quantitative Determination of Dapoxetine Hydrochloride and Tadala?l in Bulk and Pharmaceutical Formulations. Journal of chromatographic science. 2020; 58(4) : 303-308.

12- Basma H. Anwar, Nessreen S. Abdelhamid, Maimana A. Magdy and Ibrahim A. Naguib. Linear Support Vector Regression and Partial Least-Squares for Determination of Dapoxetine Hydrochloride and Tadalafil in Binary Pharmaceutical Mixtures. Journal of AOAC INTERNATIONAL. 2020;103(1) .

13- Ibrahim A. Naguib, Nessreen S. Abdelhamid, Basma H. Anwar and Maimana A. Magdy. Three Spectrophotometric Methods for Quantitative Analysis of Duloxetine in Presence of its Toxic Impurity: 1-Naphthol. Journal of AOAC INTERNATIONAL. 2020; 103(4) :  972–979.

14- Nessreen S. Abdelhamid. A comparative study of two novel validated spectrophotometric techniques for resolution of four- component mixtures with severely overlapping spectra. Spectrochimica Acta Part A. 2020; 233: 118213.

15- Nehal F. Farid, Ibrahim A. Naguib, Nessreen S. Abdelhamid, Basma H. Anwar and Maimana A. Magdy . Validated ecofriendly chromatographic method for quantitative determination of anti-migraine quaternary mixture. Journal of separation science. 2020; 43(12) : 2330-2337.

16- Nessreen S. Abdelhamid, Ibrahim A. Naguib, Basma H. Anwar and Maimana A. Magdy . A validated HPTLC method for quantitative determination of Duloxetine hydrochloride and 1-naphthol in bulk and pharmaceutical formulation. JPC-Journal of planar chromatography-Modern TLC. published 23 July 2020.

17- Eglal A. Abdelaleem, Dalal A. Abou El Ella, Alaa M. Mahmoud , Nessreen S. Abdelhamid. Green analysis of newly approved binary omeprazole / aspirin mixture in presence of aspirin Impurity using ultra high performance liquid chromatography and TLC methods. Journal of biomedical chromatography. Accepted 31 August 2020.

 

Reviewer in some scientific journals

  • Spectrochimica Acta
  • Journal of Planar Chromatography
  • Analytical Chemistry letters
  • Journal of Drug Research And Development
C.V PDF

Master Title

Analytical study of some drugs affecting respiratory system

Master Abstract

The thesis includes a general introduction about the respiratory system and the drugs affecting it. In addition it contains three parts concerning the determination of diphenhydramine hydrochloride/ menthol mixture by gas chromatography (GC); UV- spectrophotometry and colorimetry as well as doxycycline hyclate/ ambroxol hydrochloride mixture by direct ; first derivative, first derivative of ratio spectrophotometry and spectrodensitometry. Oxeladine citrate was determined in presence of its oxidative degradate a,a -diethylbenzeneacetic acid and the two preservatives methylparaben and propylparaben by second derivative spectrophotometry and multivariate manipulation of the spectrophotometric data. All these techniques where applied to the drugs in pure forms and in pharmaceutical dosage forms. This thesis is concerned with analytical study of some drugs affecting the respiratory system representing different chemical classes namely diphenhydramine hydrochloride, menthol, doxycycline hydrochloride in the hyclate form, ambroxol hydrochloride and oxeladine citrate. The aim of this work was the development of analytical methods which would be feasible, simple, rapid, sensitive and selective for determination of diphenhydramine hydrochloride /menthol mixture, doxycycline hydrochloride /ambroxol hydrochloride mixture and oxeladine citrate in presence of its oxidative degradate a,a -diethylbenzeneacetic acid and the two preservatives methylparaben and propylparaben in pure forms and the the adaptation of these methods to the available pharmaceutical dosage forms. Different analytical techniques were applied in this thesis including; direct spectrophotometry, first and second derivative spectrophotometry , first derivative of the ratio spectra, colorimetry, spectrodensitometry, gas chromatography and chemometric manipulation of the spectrophotometric data. The aim was achieved by studying the conditions of degradation for some of these drugs and isolation of the corresponding degradation products, followed by the elucidation of their structures. The isolated degradates were subsequently used for the development of stability indicating analytical methods. This thesis is composed of four parts: Part I: GENERAL INTRODUCTION This part includes a brief idea about classification pharmacology and mechanisms of actions of drugs affecting the respiratory system. PART II: SIMULTANEOUS DETERMINATION OF DIPHENHYDRAMINE HYDROCHLORIDE AND MENTHOL IN PURE FORM AND PHARMACEUTICAL PREPARATION. This part includes a general introduction about the chemistry and the mode of actions of diphenhydramine hydrochloride and menthol followed by representation of the reported methods for their quantitative analysis. Experimental results and discussion are also given. This part contains three sections: Section (A): Simultaneous Determination Of Diphenhydramine Hydrochloride And Menthol By Gas Chromatographic Method. In this section a GC method was applied which utilizes Nitrogen as a carrier gas at a flow rate of 25 cm3/min adjusting the column temperature programming to be (from 70 to 225?C at a rate of 10?C / min using a flame ionization detector adjusted at 250?C. Two peaks were obtained for diphenhydramine hydrochloride (Rt=15.51min) and menthol (Rt=6.2min). The sensitivity ranges were 10-60 and 10-40 µg/mL for the two drugs, respectively, with mean percentage recoveries of 99.25±0.664% and 100.45±0.634% respectively. The selectivity of the method was checked by using different laboratory prepared mixtures. It was successfully applied to the dosage form and the accuracy was checked by application of standard addition technique. Section (B): Determination Of Diphenhydramine Hydrochloride In Presence Of Menthol By The Direct Spectrophotometric Method. This method depends on the direct measurement of the absorbance of diphenhydramine hydrochloride at 258 nm as menthol has no absorbance in the UV-visible region . The sensitivity range was 5-20 µg/mL with mean percentage recovery of 101.03±0.466%. The selectivity of the method was checked by using different laboratory prepared mixtures. It was successfully applied to the dosage form and the accuracy was checked by application of standard addition technique. Section (C): Determination Of Menthol In Presence Of Diphenhydramine Hydrochloride By Colorimetric Method. In this section a colorimetric method was applied with the use of a solution of 1% vanillin in concentrated sulfuric acid to give a blue color measured at 619nm. The sensitivity range was 5-30 µg/mL with mean percentage recovery of 100.26±0.859%. The selectivity of the method was checked by using different laboratory prepared mixtures. It was successfully applied to the dosage form and the accuracy was checked by application of standard addition technique. PART III: SIMULTANEOUS DETERMINATION OF DOXYCYCLINE HYDROCHLORIDE HYCLATE AND AMBROXOL HYDROCHLORIDE IN PURE FORM AND PHARMACEUTICAL PREPARATION. This part includes a general introduction about the chemistry and the mode of actions of doxycycline hyclate and ambroxol hydrochloride followed by presentation of the reported methods for their qualitative analysis. Experimental results and discussion were also given. This part contains three sections: Section (A): Simultaneous Determination Of Doxycycline Hyclate And Ambroxol Hydrochloride By The Spectrophotometric Method In The Presence Of The Oxidative Degradate Of Ambroxol (4-[(2- Amino -3,5- dirombenzyl) amino] cyclohexanone). This section presents a spectrophotometric method which depends on the direct measurement of the absorbance of doxycycline hyclate at ?max 359 .8 nanometer as both ambroxol and it's oxidative degradate have no absorbance in the wavelengths above 350 nm. The sensitivity range was 7-30 µg/mL with mean percentage recovery of 100. 92 ± 0.491%. As for ambroxol it was analyzed by measuring the D1 amplitude value at 296.2 nm which is a zero crossing point for both the degradate and doxycycline. The sensitivity range was 7-30 µg/mL with mean percentage recovery of 98. 98±0.659 %. The selectivity of the method was checked by using different laboratory prepared mixtures. It was successfully applied to the dosage form and its accuracy was checked by application of standard addition technique. Section (B): Simultaneous Determination Of Doxycycline Hyclate And Ambroxol Hydrochloride By The First Derivative Of The Ratio Spectrophotometric Method. This method depends on applying the first derivative of the ratio Spectra (1DD) technique with measurement of the amplitude value of Doxycycline at 229 nm, using the spectrum of Ambroxol ( 7 µg/mL) as a divisor where it showed no interference the sensitivity range was (7 - 25 µg/mL ) microgram per mille with mean percentage recovery of 98.80±0.408%. while for ambroxol analysis, the amplitude was measured at 292.6 and 327.2 nm, using the spectrum of Doxycycline (9 µg/mL) as a divisor. The sensitivity ranges were (7-27µg/mL) for both wavelengths, with mean percentage recoveries of 98.63 ±0.304%and 99.61 ± 0.847 %) for the two wavelengths, respectively. The selectivity of the methods was checked by using different laboratory prepared mixtures. The method was successfully applied to the dosage form and the accuracy was checked by application of standard addition technique. ?Section (C): Determination Of Doxycycline Hyclate And Ambroxol Hydrochloride By The Spectrodensitometric Method. In this section both drugs are separated on a silica gel plate using n-butanol: water :acetic acid (7:3:3 ,by volume) as a developing system and UV detection at 254nm over concentration range of (2 - 12 µg/band for both drugs with mean percentage recoveries of 100. 12±0.821% and 100.31±1.334% for doxycycline( Rf=0.63) and ambroxol (Rf=0.83), respectively. The selectivity of the method was checked by using different laboratory prepared mixtures. The method was successfully applied to the dosage form and the accuracy was checked by application of standard addition technique. PART IV: STABILITY INDICATING METHODS FOR THE DETERMINATION OF OXYGEN CITRATE IN PRESENCE OF ITS HYDROLYTIC DEGRADED AND EACH OF METHYLPARABEN AND PROPYLPARABEN IN PURE FORM AND PHARMACEUTICAL PREPARATIONS. This part includes a general introduction about the chemistry and mode of action of oxeladine citrate, followed by presentation of the reporting methods for its qualitative analysis. Experimental results and discussions were also given. The hydrolytic degradation pathway of the drug was also presented, followed by the method of separation of the drug and its degradate. This part contains 2 sections: Section (A): Application Of Second Derivative Spectrophotometric Method As A Stability Indicating Method For The Determination Of Oxeladine Citrate In Presence Of Its Degradate And The Two Preservatives Methylparaben And Propylparaben. This section presents a D2 spectrophotometric method which depends on the measurement of the peak amplitude of oxeladine citrate at 227.4nm, which is a zero crossing point for the degradate a, a diethylbenzene acetic acid. The interference of the two preservatives methylparaben and propylparaben present in the syrups was overcome by extracting the two preservatives from the syrups by ethyl acetate, in which oxeladine citrate is insoluble. The sensitivity range was 10-40 µg/mL with mean percentage recovery of 100.12±0.363%. The selectivity of the method was checked by using different laboratory prepared mixtures. It was successfully applied to the dosage form and its accuracy was checked by application of standard addition technique. Section (B): Application Of The Multivariate Spectrophotometric Methods As Stability Indicating Methods For The Determination Of Oxeladine Citrate In Presence Of Is Degradate And The Two Preservatives MP And PP. The chemometric techniques;Classical least squares (CLS), Principal component regression (PCR) and Partial least squares (PLS), have been successfully applied for the determination of oxeladine citrate in presence of its degradate and the two preservatives MP and BP. A training set of 12 mixtures containing different ratios of the four drugs is used. The selectivity of the methods was checked using laboratory prepared mixtures (a validation set consisting of 8 mixtures). It was successfully applied for the determination of oxeladine citrate in its different syrup formulations. The validity of the methods was assessed by application of the standard addition technique.

Master Abstract PDF

PHD Title

Analytical Study Of Some Pharmaceutical Compounds Acting On The Respiratory System

PHD Abstract

This thesis is concerned with analytical study of some pharmaceutical compounds acting on the respiratory system namely; Diphenhydramine HCl (DH), its mixture with Paracetamol (PC) and Oxeladin Citrate (OL), The aim of this work is to develop new simple, rapid, sensitive and selective methods for the determination of the cited drugs in their mixtures and in presence of their different degradates and common interfering additives either in bulk forms or in pharmaceutical formulations. Different analytical techniques are adopted in this thesis including; derivative spectrophotometry, second derivative of the ratio spectra spectrophotometry, isoabsorptive point spectrophotometry, ratio subtraction spectrophotometry,mean centering spectrophotometry, double divisor spectrophotometry, TLC-densitometry, high performance liquid chromatography and multivariate calibration of spectrophotometric data. The thesis consists of four parts: PART I :General introduction This part includes a simple pharmacological introductionabout drugs acting on the respiratory system and their classification, followed by a general introduction about the chemistry of the studied drugs, their physical properties, modes of action and the literature review concerning their reported methods of analysis. PART II :Stability indicating spectrophotometric methods for determination of Diphenhydramine hydrochloride in presence of its N-oxide derivative. This part includes the forced degradation and stability study of diphenhydramine hydrochloride, accompanied by the method of preparation and identification of its N-oxide derivative, followed by five different stability indicating techniques suggested forthe determination ofdiphenhydramine hydrochloride in presence of its N-oxide derivative. This part consists of six sections: Section A :Degradation and stability study of Diphenhydramine hydrochloride This section discusses the stability study ofdiphenhydramine hydrochloride under stress degradation conditions including acid hydrolysis, alkaline hydrolysis, oxidation and photolysis using white cool lamp and UV lamp. This section illustrates the oxidation pathway of diphenhydramine hydrochloride degradation, the method of preparation of the pure N-oxide derivative and its identification using IR and mass spectra. Section B :Stability indicating third derivative spectrophotometric method for determination of Diphenhydramine hydrochloride in presence of its N-oxide derivative. In this section diphenhydramine hydrochloride was determined using the third derivative spectrophotometric method in presence of its N-oxide derivative by measuring the peak amplitude at 281 nm, which is a zero crossing point (ZCP) of the derivative. The amplitude was linear with the concentration over a range of 3-35 µgmL-1. The selectivity of the method was checked by analyzing diphenhydramine hydrochloride concentration in different laboratory prepared mixtures containing different ratios of the drug and its N-oxide derivative.The method was successfully applied to Sultan® capsules with no interference from additives.The accuracy of the method was assured by applying the standard addition technique to the capsules. The results of the method were statistically compared with the pharmacopoeial HPLC method, where the obtained t and F values were found to be less than the tabulated ones, indicating no significant difference with respect to accuracy and precision. Section C :Stability indicating second derivative of the ratio spectra spectrophotometric method for determination of Diphenhydramine hydrochloride in presence of its N-oxide derivative. In this section diphenhydramine hydrochloride was determined using the second derivative of the ratio spectra spectrophotometric method in presence of itsN-oxide derivative by measuring the peak amplitude at 274.5 nm, which is a zero crossing point (ZCP) of the N-oxide derivative. The spectrum of 20µgmL-1 solution of the N-oxide derivative was used as a divisor. The amplitude was linear with the concentration over a range of 10-35 µgmL-1. The selectivity of the method was checked by analyzing diphenhydramine hydrochloride concentration in different laboratory prepared mixtures containing different ratios of the drug and its N-oxide derivative. The method was successfully applied to Sultan® capsules with no interference from additives.The accuracy of the method was assured by applying the standard addition technique to the capsules. The results of the method were statistically compared with the pharmacopoeial HPLC method, where the obtained t and F values were found to be less than the tabulated ones, indicating no significant difference with respect to accuracy and precision. Section D :Stability indicating isoabsorptive point spectrophotometric method for determination of Diphenhydramine hydrochloride in presence of its N-oxide derivative. In this section diphenhydramine hydrochloride was determined using the isoabsorptive point spectrophotometric method in presence of itsN-oxide derivative by measuring the absorbance at 226 nm, which is the isoabsorptive point of the drug and its N-oxide derivative. At this point the total concentration of the mixture was considered as diphenhydramine hydrochloride. The concentration of the N-oxide derivative is calculated by measuring its absorbance at 271 nm , which is its ?max, then the concentration of diphenhydramine hydrochloride is calculated by subtraction. The absorbance was linear with the concentration over a range of 2-50 µgmL-1. The selectivity of the method was checked by analyzing diphenhydramine hydrochloride concentration in different laboratory prepared mixtures containing different ratios of the drug and its N-oxide derivative. The method was successfully applied to Sultan® capsules with no interference from additives.The accuracy of the method was assured by applying the standard addition technique to the capsules. The results of the method were statistically compared with the pharmacopoeial HPLC method, where the obtained t and F values were found to be less than the tabulated ones, indicating no significant difference with respect to accuracy and precision. Section E :Stability indicating ratio subtraction spectrophotometric method for determination of Diphenhydramine hydrochloride in presence of its N-oxide derivative. In this section diphenhydramine hydrochloride was determined using the ratio subtraction spectrophotometric method in presence of itsN-oxide derivative. The interference of the degradate is removed by dividing the spectra of the mixtures by the spectrum of 20µgmL-1 solution of the N-oxide derivative, then subtracting the resulting plateau and finally re-multiplication by the same divisor The amplitude of diphenhydramine hydrochloride at 207 nm was linear with the concentration over a range of 2-30 µgmL-1. The selectivity of the method was checked by analyzing diphenhydramine hydrochloride concentration in different laboratory prepared mixtures containing different ratios of the drug and its N-oxide derivative. The method was successfully applied to Sultan® capsules with no interference from additives.The accuracy of the method was assured by applying the standard addition technique to the capsules. The results of the method were statistically compared with the pharmacopoeial HPLC method, where the obtained t and F values were found to be less than the tabulated ones, indicating no significant difference with respect to accuracy and precision. Section F :Stability indicating mean centering spectrophotometric method for determination of Diphenhydramine hydrochloride in presence of its N-oxide derivative. In this sectiondiphenhydramine hydrochloride was determined using the mean centering spectrophotometric method in presence of its N-oxide derivative, where the interference of the N-oxide derivative is removed by dividing the spectra of the mixtures by the spectrum of 20µgmL-1 solution of the degradate, then resulting spectrum is mean centered. The concentration of diphenhydramine hydrochloride is calculated by measuring the amplitude at 280 nm, which was found to be linear with the concentration over a range of 2-45 µgmL-1. The selectivity of the method was checked by analyzing diphenhydramine hydrochloride concentration in different laboratory prepared mixtures containing different ratios of the drug and its N-oxide derivative. The method was successfully applied to Sultan® capsules with no interference from additives.The accuracy of the method was assured by applying the standard addition technique to the capsules. The results of the method were statistically compared with the pharmacopoeial HPLC method, where the obtained t and F values were found to be less than the tabulated ones, indicating no significant difference with respect to accuracy and precision. The results obtained from the five proposed methods were compared together and to the official method using one way ANOVA test where no significant differences were found. PART III :Simultaneous determination of Paracetamol and Diphenhydramine hydrochloride in presence of their degradates p-aminophenol and diphenhydramine N-oxide derivative This part includes three different stability indicating techniques suggested forthe simultaneous determination ofparacetamol and diphenhydramine hydrochloride in presence of their degradates; p-aminophenol the hydrolytic degradate of paracetamol and one of its most common impurities and the N-oxide N-oxide derivative of diphenhydramine hydrochloride. This part consists of three sections: Section A :Double divisor spectrophotometric method for simultaneous determination of Paracetamol and Diphenhydramine hydrochloride in presence of their degradates In this section the double divisor method has been used for the simultaneous determination of paracetamol and diphenhydramine hydrochloride in presence of their degradation products p-aminophenol and the N-oxide derivative of diphenhydramine hydrochloride.The interference caused by the two degradates was removed by dividing the spectra of the analyzed drugs or quaternary mixtures by the spectrum of a mixture containing equal concentrations of the two degradates. The second derivative of the resulting spectra was obtained. Paracetamol was determined by measuring theamplitude at 304 nm, where the contribution ofDiphenhydramine hydrochloride is zero. The amplitude was linear with the concentration over a range of 2-45 µgmL-1. Diphenhydramine hydrochloride was determined by measuring the amplitude at 256.4 nm, which is a ZCP for paracetamol. The amplitude was linear with the concentration over a range of 2-45 µgmL-1. The selectivity of the method was checked by analyzing paracetamol and diphenhydramine hydrochloride in different laboratory prepared mixtures containing different ratios of the 4 components. The method was successfully applied to Panadol night® tablets with no interference from additives.The accuracy of the method was assured by applying the standard addition technique to the tablets. The results of the method were statistically compared with the pharmacopoeial HPLC method, where the obtained t and F values were found to be less than the tabulated ones, indicating no significant difference with respect to accuracy and precision. Section B :Multivariate calibration method for simultaneous determination of Paracetamol and Diphenhydramine hydrochloride in presence of their degradates In this section two chemometric techniques; Principle component regression (PCR) and Partial least square (PLS) have been successfully applied for the simultaneous determination of paracetamol and diphenhydramine hydrochloridein their quaternary mixtures with their degradates either in bulk forms or in pharmaceutical formulation. The two models were constructed using 13 mixtures containing different concentrations of the four components. The selectivity of the method was checked by analyzing paracetamol and diphenhydramine hydrochloride concentration in different laboratory prepared mixtures (a validation set consisting of 12 mixtures). The method was successfully applied to Panadol night® tablets with no interference from additives.The accuracy of the method was assured by applying the standard addition technique to the tablets. Section C :TLC-densitometric method for simultaneous determination of Paracetamol and Diphenhydramine hydrochloride in presence of their degradates In this section the TLC-densitometric method has been used for the simultaneous determination of paracetamol and diphenhydramine hydrochloride in presence of their degradation products p-aminophenol and the N-oxide derivative of diphenhydramine hydrochloride. The 4 components were separated on silica gel plates using a developing system consisting of ethyl acetate - acetone -20%methanolic sodium lauryl sulphate - acetic acid (5:5:1:0.25 by volumes). Peaks were detected at 254 nm. The four separated components had different Rf values; paracetamol (0.87), diphenhydramine hydrochloride (0.11), p-aminophenol (0.65) andN-oxide derivative of diphenhydramine hydrochloride (0.33).The method is applicable over concentration ranges of (1-60µg band-1) for paracetamol and (1-30µg band-1) for diphenhydramine hydrochloride The method was successfully applied to Panadol night® tablets with no interference from additives.The accuracy of the method was assured by applying the standard addition technique to the tablets. The results of the method were statistically compared with the pharmacopoeial HPLC method, where the obtained t and F values were found to be less than the tabulated ones, indicating no significant difference with respect to accuracy and precision. The results obtained from the three proposed methods were compared together and to the official method using one way ANOVA test where no significant differences were found. PART IV :Determination of Oxeladin citrate in presence of its hydrolytic degradate, its N-oxide derivative and the two preservatives methyl paraben and propyl paraben This part includes the forced degradation and stability study of oxeladin citrate, accompanied by the method of preparation and identification of its alkaline induced hydrolytic degradate and its N-oxide derivative, followed by three different stability indicating techniques suggested forthe determination of oxeladin citrate in presence of its two different degradates and the two preservatives methyl paraben and propyl paraben. This part consists of four sections: Section A :Degradation and stability study of Oxeladin citrate This section discusses the stability study of oxeladin citrate under stress degradation conditions including acid hydrolysis, alkaline hydrolysis, oxidation and photolysis using white cool lamp and UV lamp. This section illustrates both the alkaline induced hydrolytic and the oxidation pathways of oxeladin citrate degradation and the method of preparation of pure degradation products and their identification using IR and mass spectra. Section B :Multivariate calibration methods for determination of Oxeladin citrate in presence of its hydrolytic degradate, its N-oxide derivative and the two preservatives Methyl paraben and Propyl paraben. In this section two chemometric techniques; Principle component regression (PCR) and Partial least square (PLS) have been successfully applied for the determination of oxeladin citrate in presence of its two degradates and the two preservatives methyl paraben and propyl paraben either in bulk forms or in pharmaceutical formulations. The two models were constructed using 12 mixtures containing different concentrations of the five components. The selectivity of the method was checked by analyzing oxeladin citrate concentration in different laboratory prepared mixtures (a validation set consisting of 13 mixtures). The method was successfully applied to Oxeladine® and Paxeladine® syrups with no interference from other additives. The accuracy of the method was assured by applying the standard addition technique to the syrups. Section C :High performance liquid chromatographic method for determination of Oxeladin citrate in presence of its hydrolytic, its N-oxide derivative and the two preservatives Methyl paraben and Propyl paraben. In this section a RP-HPLC method has been used for the separation and determination of oxeladin citrate in presence of its 2 degradation products and the two preservatives methyl paraben and propyl paraben. The 5 components were separated on a C18 column using a mobile phase consisting of methanol /water (1:1, maintained at pH=3 by trifluoroacetic acid)at a flow rate of 2 mL min-1 and detected at 220 nm.The five separated components had different tR values; oxeladin citrate (2.6 min), the N-oxide derivative (6.2 min), the hydrolytic degradate (13.7 min) andthe two preservatives at the same tR value(9.3 min). The method is applicable over a concentration range of (5-200µg band-1) of oxeladin citrate.The method was successfully applied to Oxeladine® and Paxeladine® syrups with no interference from other additives.The accuracy of the method was assured by applying the standard addition technique to the syrups. The results of the method were statistically compared with the reported HPLC method, where the obtained t and F values were found to be less than the tabulated ones, indicating no significant difference with respect to accuracy and precision. Section D :TLC-densitometric method for determination of Oxeladin citrate in presence of its hydrolytic degradate, its N-oxide derivative and the two preservatives Methyl paraben and Propyl paraben. In this section the TLC-densitometric method has been used for the determination of oxeladin citrate in presence of its two degradation products and the two preservatives methyl paraben and propyl paraben. The 5 components were separated on silica gel plates using a developing system consisting of acetone- ethyl acetate -7%methanolic sodium lauryl sulphate - acetic acid (6:5:3:0. 5 by volumes). Peaks were detected at 220 nm. The five separated components had different Rf values;oxeladin citrate (4.2), the N-oxide derivative (0.71), the hydrolytic degradate (0.19) andthe two preservatives had the same Rf value (0.87). The method is applicable over a concentration range of (0.1-2µg band-1) of oxeladin citrate The method was successfully applied to Oxeladine® and Paxeladine® syrups with no interference from other additives.The accuracy of the method was assured by applying the standard addition technique to the syrups. The results of the method were statistically compared with the reported HPLC method, where the obtained t and F values were found to be less than the tabulated ones, indicating no significant difference with respect to accuracy and precision. The results obtained from the three proposed methods were compared together and to the official method using one way ANOVA test where no significant differences were found. This thesis contains 164 references, 67 figures and 70 tables and ends with an Arabic summary.

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