الفهرس 
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Abstract
ABSTRACT
Name: Ahmed Salah Abdalla Ali Mansour
Title of the thesis: Development and validation of chromatographic method for analysis of some azole compounds in pharmaceutical formulation.
Degree: master of Science in nonorganic chemistry (Analytical Chemistry)
This study presents the development, optimization and validation of simple HPLC methods for the determination of different pharmaceutical products specially ((Azoles compounds)). The developed methods were presented as follows:
1. Metronidazole and nystatin method of analysis, which contains novel and validated HPLC method that applied for the simultaneous determination of metronidazole and nystatin in bulk and in pharmaceutical formulation. chromatographic determination of the two drugs was performed on XBridge phenyl column (250 mm x 4.6 mm, 3.5 µm particle size) and UV detection was carried at 380 nm for the first 4.5 minutes then the detection was done at 305 nm to end of the run. A mobile phase comprising methanol, acetonitrile, and 0.01 mol L-1 sodium acetate adjusted to pH 4.2 with glacial acetic acid in a ratio of 70:5:25 (v/v/v) was used for the separation of metronidazole and nystatin by an isocratic elution technique. Injection volume: 20 µL, flow rate: 1 mL min-1 and temperature 30˚C.
2. Domperidone and esomeprazole method of analysis, which contains novel and validated HPLC method that applied for the simultaneous determination of domperidone and esomeprazole in bulk and in pharmaceutical formulation. Symmetry C18 column (250 mm x 4.6 mm, 5.0 µm particle size) using an isocratic elution technique and UV detection at 290 nm. Total elution program was 7 min and a mobile phase consisting of 0.01 mol L-1 sodium acetate buffer (pH 4.5): methanol was used with a ratio of 45:55 (v/v) at a flow rate of 1.3 mL min-1. Injection volume: 20 µL, temperature 30˚C.
3. Metronidazole, fluconazole, and voriconazole method of analysis, which contains novel and validated HPLC method that applied for the simultaneous determination of metronidazole, fluconazole, and voriconazole in bulk and in their cream mixture. Hypersil BDS C18 Column (250 x 4.6 mm, 5 µm) was used with gradient elution mode and UV detection was done at 360 nm. Total elution program was 23 min and a mobile phase consisting of 0.01 mol L-1 sodium acetate buffer (pH 5.5): acetonitrile: methanol was utilized with a ratio of 70:20:10 (v/v/v) for the first 7 min at a flow rate of 1.0 mL min-1 then with a ratio of 50:20:30 (v/v/v) at a flow rate of 1.5 mL min-1 for the next 11 minutes. Finally, the gradient program was returned to the initial conditions and the analytical column was reconditioned for 5 minutes. Injection volume: 50 µL, temperature 30˚C.
These methods were validated as per ICH guidelines. The methods showed good linearity, limit of detection, limit of quantification, accuracy, precision, ruggedness, and robustness. The methods were suitable for routine analysis of the investigated drugs individually and in their combined dosage forms; and also suitable as stability indicating methods.
Keywords: HPLC, Validation, Metronidazole, Nystatin, Domperidone, Esomeprazole, Metronidazole, Fluconazole, Voriconazole