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العنوان
Analytical study of selected multi-component mixtures in pharmaceutical preparations /
المؤلف
Abdel-Fatah, Amany Abdel-Aziz Khalil.
هيئة الاعداد
باحث / أماني عبد العزيز خليل عبد الفتاح
مشرف / هشام سالم شرف الدين
مشرف / محمود أحمد عمر
مشرف / سيد محمد سيد دريع
الموضوع
Chemistry, Analytic.
تاريخ النشر
2019.
عدد الصفحات
137 p. :
اللغة
الإنجليزية
الدرجة
ماجستير
التخصص
الصيدلة ، علم السموم والصيدلانيات
تاريخ الإجازة
1/1/2019
مكان الإجازة
جامعة المنيا - كلية الصيدلة - الكيمياء التحليلية
الفهرس
Only 14 pages are availabe for public view

from 160

from 160

Abstract

This thesis consists of four parts:
Part I
General introduction
This part provided a general introduction about the chemistry, mode of action, literature review of the reported analytical methods and scope of investigation.
Part II
Thin layer-chromatographic methods
This part is divided into three chapters:
Chapter 1: Simultaneous determination of binary mixture of Cinchocaine HCl and Policresulen in dosage forms by Thin-Layer chromatography–Spectro densitometry.
TLC-spectrodensitometric method was developed and validated for the simultaneous determination of PC and CIN. The spectrodensitometric method was based on separation of both drugs on TLC aluminum plates of silica gel 60 F254, using chloroform: methanol: ammonia (9.5:0.6:1.0, v/v/v) as a mobile phase and Dragendorff reagent as spot detection at 490 nm. The SD was 1.1±0.03 and 0.49 ±0.03 for PC and CIN, respectively.
Chapter 2: Simultaneous determination of ternary mixture of Mometasone furoate, Miconazole nitrate and Gentamicin in dosage form by Thin-Layer chromatography–Spectrodensitometry.
TLC-spectrodensitometric method was developed and validated for the simultaneous determination of MF, MIC, and GM. The spectrodensitometric method was based on separation of drugs using chloroform: methanol: formic acid (4:0.3:0.15, v/v/v) as a mobile phase. Quantification was carried out with UV detection at 254 nm. The SD was 1.48±0.03, 0.34±0.03, and 0.97±0.03 for MF, MIC, and GM respectively.
Chapter 3: Simultaneous determination of quaternary mixture of Betamethas--one valerate, Tolnaftate, Gentamicin, and Clioquinol in dosage form by Thin-Layer chromatography– Spectrodensitometry.
TLC-spectrodensitometric method was developed and validated for the simultaneous determination of BV, TF, GM, and CQ. The spectrodensitometric method was based on separation of drugs using chloroform: methanol: acetic acid: formic acid (6:1:0.15:0.25, v/v/v) as a mobile phase. Quantification was carried out with UV detection at 254 nm. The SD was 0.87±0.03 ,0.42±0.03 ,0.56±0.03, and 0.43±0.03 for BV, TF, GM and CQ, respectively.
The proposed methods were validated according to ICH guidelines and was applied for the simultaneous determination of the cited drugs in synthetic mixtures and pharmaceutical preparations. The methods were successfully applied for the routine analysis of cited drugs with no need for prior separation. The results obtained were statistically compared with that of the reported and official methods. The statistical comparison showed that there is no significant difference regarding both accuracy and precision.
Part III
Multi-variate chemometric methods
This part is divided into two chapters:
Chapter 1: Simultaneous determination of ternary mixture of Mometasone furoate, Miconazole nitrate, and Gentamicin in dosage form by multi-variate chemometric methods.
The determination of this mixture was developed using two chemometric techniques; PCR and PLS. The first step in the determination of the cited drugs by multivariate calibration method involved constructing the calibration matrix for the ternary mixtures. The calibration set was obtained by using the absorption spectra set of fifteen concentrations of each component. In this study, the leave one out cross validation was used and the RMSECV values were used as diagnostic tests for examining the errors in the predicted concentrations. RMSECV values indicated both precision and accuracy of predictions. To validate the prediction ability of the suggested models, they were applied to estimate the concentrations of each component in the validation set of five mixtures. The two models had the same power of prediction for this mixture.
Chapter 2: Simultaneous determination of quaternary mixture of Betamethas--one valerate, Tolnaftate, Gentamicin, and Clioquinol in dosage form by multi-variate chemometric methods.
The determination of this mixture was developed using two chemometric techniques; PCR and PLS. The calibration set was obtained by using the absorption spectra set of fifteen concentrations of each component. In this study, the leave one out cross validation was used and the RMSECV values were used as diagnostic tests for examining the errors in the predicted concentrations. To validate the prediction ability of the suggested models, they were applied to estimate the concentrations of each component in the validation set of five mixtures. The two models had the same power of prediction for this mixture.
Part IV
Ion-pair complex formation
This part is divided into two parts:
Chapter 1: General introduction
This chapter provided an introduction about the reagents (Eriochrome black T, Methyl orange and chrome azurol S) and some drugs that were determined by these reagents.
Chapter 2: Colorimetric determination of Mometasone furoate and Tolnaftate by ion-pair complexes formation with Eriochrome black T, Methyl orange, and chrome azurol S.
This chapter provided the information about experiments, results and discussions about the ion-pair complexes between studied drugs (MF and TF) and the three reagents (EBT, MO, and CRS) in the concentration range of (3-15) and (1-5) μg mL−1 for MF and TF, respectively. The SD was 1.39±0.03 ,1.41±0.03 ,1.22±0.03, 0.73±0.03, 1.42±0.03, and 0.34±0.03 for (MF-EBT), (MF-MO), (MF-CRS), (TF-EBT), (TF-MO), and (TF-CRS), respectively. The results obtained were statistically compared with that of the reported methods. The statistical comparison showed that there is no significant difference regarding both accuracy and precision.