Unit:
Κατεύθυνση Φαρμακευτική Ανάλυση - Έλεγχος ποιότηταςLibrary of the School of Science
Author:
Sourtzi Evangelia
Supervisors info:
Μιχαήλ Κουππάρης, Καθηγητής, Τμήμα Χημείας, ΕΚΠΑ
Original Title:
Ανάπτυξη και επικύρωση μεθόδων HPLC για τον ποσοτικό προσδιορισμό δικλοφαινάκης, θειοκολχικοσίδη και των συγγενών ουσιών τους σε δερματικό διάλυμα
Translated title:
Development and validation of HPLC methods for the determination of diclofenac, thiocolchicoside and their related substances in cutaneous solution
Summary:
The purpose of this MSc Thesis is the development and validation of analytical methods for the determination of the active substances diclofenac sodium and thiocolchicoside and their related substances in cutaneous solution, using High Performance Liquid Chromatography with PDA detector.
Diclofenac sodium is a nonsteroidal anti-inflammatory drug (NSAID), which is widely used in topical formulations. A selective and reproducible analytical method, for the simultaneous determination of diclofenac sodium and its related substances, was developed. Separation was performed isocratically on a C18 (250×4.6 mm, 5 μm) column, with a mobile phase consisting of phosphate buffer pH 2.5 - methanol (34:66 v/v) at flow rate 1.0 mL/min. The detection was carried out at 254 nm. The limit of detection was found to be 0.012 μg/mL and the quantitation limit 0.036 μg/mL.
Thiocolchicoside, which is not included in the European Pharmacopoeia, is a muscle skeletal relaxant and is also used in topical formulations. The determination was performed isocratically on an Hypersil Silica (250×4.6 mm, 5 μm) column, with a mobile phase consisting of chloroform – methanol (85:15 v/v) at flow rate 1.0 mL/min. The detection was carried out at 370 nm and the column temperature was set at 30 οC. Gradient elusion was performed for the determination of the impurities, with the same chromatographic parameters. The limits of detection ranged from 1.9 to 3.5 ng/mL and the quantitation limits from 5.7 to 10.6 ng/mL.
The developed analytical methods were validated according to International Guidelines (ICH Guidelines), after examining and evaluating quality characteristics, such as linearity, precision, accuracy, robustness and detection and quantitation limits.
Main subject category:
Science
Other subject categories:
Pharmacy
Keywords:
Diclofenac, Thiocolchicoside, Related substances, Validation, HPLC
Number of index pages:
13-16
