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العنوان
Analytical Study on Certain Fluorinecontaining Drugs /
المؤلف
Trabik,Yossra Ahmed Mamdouh Lotfy.
هيئة الاعداد
باحث / Yossra Ahmed Mamdouh Lotfy Trabik
مشرف / Amira Mabrouk El-Kosasy
مشرف / Lobna Abdel-Aziz Hussein
تاريخ النشر
2016
عدد الصفحات
321p.;
اللغة
الإنجليزية
الدرجة
الدكتوراه
التخصص
العلوم الصيدلية
تاريخ الإجازة
1/1/2016
مكان الإجازة
جامعة عين شمس - كلية الصيدلة - العلوم الصيدلية
الفهرس
Only 14 pages are availabe for public view

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Abstract

This thesis consisted of five parts:
Part I: General introduction
It explained the nature of fluorine-containing drugs, and their increased
introduction into the pharmaceutical field.
Part II: Literature review
This part included a review of the physical and chemical properties of the studied
fluorine-containing drugs, Rosuvastatin calcium, Fluticasone propionate, and
Sodium fluoride. Also, it included different analytical methods reported in the
literature that aimed for determination of the chosen drugs in pure form, mixtures,
pharmaceutical formulations, and biological fluids.
Part III: Spectrophotometric determination of fluorinecontaining drugs
This part involved the development of ratio derivative, ratio difference and mean
centering procedures for analysis of Rosuvastatin calcium, as well as Area under
curve and Savitsky-Golay filter procedures for analysis of Fluticasone propionate,
with further application to mixtures, pharmaceutical formulations and urine
samples. This part was divided into three sections:
Section A: Ratio derivative and ratio difference methods for
determination of Rosuvastatin in presence of Losartan
The ratio derivative method was utilized to determine Rosuvastatin. The peak
amplitude of Rosuvastatin at 237.00 nm from the ratio derivative spectrum (using
Losartan 1 µg/ml as a divisor) was measured. In ratio difference method, the
amplitude difference of the ratio spectra (RSV/LOS) at 215.30 and 309.50 nm
(ΔP309.50-215.30) was utilized to determine Rosuvastatin without any
interference from Losartan. The methods were applied for the determination of Rosuvastatin in its pure form, in presence of Losartan, and in their urine samples
with good accuracy and recovery.
Section B: Mean centering method for determination of
Rosuvastatin in presence of Losartan and Metformin
The mean centering method was utilized to selectively quantify Rosuvastatin.
Rosuvastatin was measured at 250.80 nm from the second-mean centered ratio
spectrum (using Losartan and Metformin 1 µg/ml as a divisor). Rosuvastatin was
determined in bulk powder, pharmaceutical formulation, and in presence of
Losartan and Metformin in laboratory prepared mixtures and in urine samples.
The proposed method was easily applicable for routine analysis.
Section C: Area under curve and Savitsky-Golay Filter
methods for simultaneous determination of Fluticasone and
Salmeterol
Area under curve method was utilized to simultaneously determine Fluticasone
and Salmeterol. The values of Area under curve were measured in the range of
230.00-240.00 and 245.00-255.00 nm. In Savitsky-Golay Filter method, Peak
amplitude of Fluticasone was measured at 226.80 nm (zero-crossing of
Salmeterol). Fluticasone and Salmeterol were determined in bulk powder,
laboratory prepared mixtures, and their pharmaceutical formulation. The
proposed methods were used for routine analysis of the drugs.
Part IV: HPLC-UV determination of fluorine-containing
drugs
High Performance Liquid chromatographic techniques with UV detection were
developed for simultaneous determination of Rosuvastatin, Losartan and
Metformin as well as for simultaneous determination of Fluticasone and
Salmeterol. The proposed methods were further applied to pharmaceutical
formulation, spiked urine or plasma samples. A pre-column derivatization
reaction was developed for selective determination of Sodium fluoride and was
further applied to pharmaceutical formulations. This part involved three sections.Section A: Simultaneous determination of Rosuvastatin,
Losartan and Metformin and application to urine
This section was concerned with the application of HPLC method for the
simultaneous determination of Rosuvastatin, Losartan and Metformin. The
mobile phase of choice was acetonitrile: tri-fluoro acetic acid 0.1%
(50:50, v/v). Diode array detector was set 252.00 nm for quantitative
determination of Rosuvastatin and Losartan, and at 242.00 nm for quantitative
determination of Metformin. The proposed HPLC method was successfully
applied for determination of the mentioned drugs in pure form and laboratory
prepared mixtures. The method was further applied to simultaneous
determination of Rosuvastatin and Losartan in presence of Metformin in spiked
urine samples.
Section B: Determination of Sodium fluoride using precolumn derivatization reaction and application to
pharmaceutical formulations
This section was concerned with the application of HPLC method for the
selective determination of Sodium fluoride. A pre-column derivatization reaction,
utilizing triphenyl silanol reagent, was developed. The reaction product,
triphenyl silyl fluoride, was aspirated and subjected to HPLC measurement. The
mobile phase of choice was acetonitrile: water (75:25, v/v). Diode array detector
was set at 222.00 nm. The proposed HPLC method was successfully applied for
determination of Sodium fluoride in pure form and pharmaceutical formulations.