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العنوان
Spectrophotometric and potentiometric determination of ketotifen fumarate drug /
المؤلف
Hwehy, Mohammad Mahmoud Abd El Fatah Mahmoud.
هيئة الاعداد
مشرف / محمد محمود عبد الفتاح محمود
مشرف / محمد مجدي خليل
مشرف / جهاد جندي محمد
الموضوع
Analytical Chemistry. Analytical Chemistry. Ketotifen fumarate. Bromothymol blue. Bromophenol blue. Eriochrome blue black R, 2,3-Dichloro-5,6-dicyanobenzoquinone. Spectrophotometry. Ion-pair formation. Pharmaceutical preparation. Potentiometry. Ion-selective electrodes.
تاريخ النشر
2012.
عدد الصفحات
102 p. :
اللغة
الإنجليزية
الدرجة
ماجستير
التخصص
Analytical Chemistry
الناشر
تاريخ الإجازة
27/10/2011
مكان الإجازة
جامعة بني سويف - كلية العلوم - الكيمياء
الفهرس
Only 14 pages are availabe for public view

from 125

from 125

Abstract

(1) Chapter I
A literature survey was presented on ketotifen fumarate drug concerning its biological activities, determination and separation at various conditions. Also it includes introduction concering the theoretical bases for preparation and uses of the different types of ion-selective electrodes, and focusing on carbon paste and PVC membrane electrodes as regards of methods of preparation and use of these surface electrodes in the potentiometric titration of KTF drug.
(2) Chapter II
Includes the experimental part. The materials, solutions, instruments used and working procedures were given. It contains full details for preparation of the carbon paste and PVC membrane electrodes and working procedures. The analytical method used in the potentiometric determination of the studied KTF drug in pure solution, in pharmaceutical preparations and urine samples is also described.
(3) Chapter III
It divided into two parts:
In the first part, simple, rapid and reliable spectrophotometric methods were adopted for the determination of KTF in both pure form and pharmaceutical preparation via ion-pair formation with bromothymol blue (BTB), bromophenol blue (BPB) and eriochrome blue black R (EBBR) reagents and formation of CT complex with 2,3-dichloro-5,6-dicyanobenzoquinine (DDQ) reagent. The second part involves potentiometric determination of KTF in both pure form pharmaceutical preparation and urine sample using carbon paste and PVC membrane electrodes.
The results obtained were divided into two parts:
(a) The first part:
Involved spectrophotometric determination of KTF drug via ion-pair formation with bromothymol blue (BTB), bromophenol blue (BPB) and eriochrome blue black R (EBBR) reagents and CT complex formation with 2,3-dichloro-5,6-dicyanobenzoquinine (DDQ) reagent.
• The optimum ratio between reactants was found to be 1:1 [drug: reagent].
• The effect of temperature on the reaction between the KTF drug and chromogenic reagents, room temperature is chosen for using BTB, BPB, EBBR and DDQ reagents.
• The complete colour development is attained after 10, 10, 5 and 5 minutes for BTB, BPB, EBBR and DDQ reagents, respectively.
• It was found that methylene chloride was the best solvent in case of BTB, BPB, EBBR and DDQ reagents, respectively.
• Universal buffer (pH=3) is found to be the best buffer in case of BTB and EBBR reagents and acetate buffer (ph=3) is suitable buffer to be used for the formation of the ion–pair with BPB reagent. The absorbance is generally increased by pH increase and reached maximum value at pH=3 with BPB and EBBR while in case of BTB reagent, the absorbance is nearly constant with pH variation.
• In the determination of KTF, Beer’s law was rectilinear in the concentration range from 1-45, 1-20, 1-10 and 10-350 μg mL-1 for KTF drug using BTB, BPB, EBBR and DDQ reagents, respectively.
Pharmaceutical preparation of KTF drug was determined spectrophotometrically using BTB, BPB, EBBR and DDQ reagents. The results obtained by the suggested procedure were compared with those obtained by the standard method. The data obtained by both procedures were found to be very close to each other and very close to those given by the pharmaceutical companies.
(b) The second part
A simple, rapid and reproducible method for production of carbon paste and PVC membrane technologies are described. The carbon paste and PVC membrane sensors were utilized as an end point indicator electrodes for the potentiometric titration of KTF drug. The preparation of the carbon paste and PVC membrane electrodes as well as the factors affecting the electrode performance with this technology are shown and discussed in details. These factors include:
1- Effect of the plasticizer type: When these electrodes are used to monitor the potentiometric titration based on ion-pair formation, o-NPOE and DOS are selected as the best plasticizer for CPE and PVC membrane, respectively.
2- Effect of the titrant: KTPB is the best titrant in case of CPE and PVC membrane electrodes.
3- Effect of the pH: pH was found to be range from 3.0 to 6.0 for CPE and from 2.0 to 7.0 for PVC membrane.
4- Effect of the temperature: The investigated CPE (DOS) and PVC (DOS) membrane electrodes were found to be usable up to 40 and 60 °C, respectively, without noticeable deviation from the Narnstian behaviour.
5- Effect of the soaking time: The electrode require 5 and 30 min soaking before application in the potentiometric titration of the drug for CPE and PVC membrane electrodes, respectively.
6- Response time: The electrodes have a very short response time reaching 4 and 12 seconds for CPE and PVC membrane electrodes, respectively.
7- Range of concentration: 10−2 to 10−7 mol L-1 for both electrodes.
The proposed electrodes have been successfully used for the potentiometric titration of KTF drug in its pure, pharmaceutical preparations and in human urine with sensitivity comparable with the spiking method.