Summary
The thesis includes four main chapters:
Chapter One: provides a general overview of some analytical methods that can be used for simultaneous determination in multicomponent mixtures and, the theory and application of those methods that are used in this work, such as the H. point standard addition method, Q-absorption ratio method, and derivative methods.
Chapter Two: Involve the simultaneous analysis of a ternary mixture containing, phenylephrine hydrochloride (PHE), chlorpheniramine maleate (CPM), and paracetamol (PAR), this procedure was conducted without prior separation and using an advanced spectrophotometric method. The H-point standard addition and absorbance correction methods were selected to determine the compounds, which are highly overlapped spectra in pharmaceutical formulations. The method is based on the use of three different wavelengths of 296 nm, 272 nm, and 227 nm for the ternary mixture. The concentration of PAR was calculated directly at 296 nm because no interferences existed. Absorbance correction method was used to remove the role of PAR at 272 nm and 227 nm. The concentrations of the PHE and CPM compounds in the mixture were determined by using the H-point standard addition method. The results showed that simultaneous determination of PAR, PHE, and CPM could be conducted within the range of 1–33 µg/mL, 1–23 µg/mL, and 1–36 µg/mL, respectively. The percent relative standard deviations for the simultaneous determination of PHE, CPM, and PAR were 0.617%, 2.76%, and 1.71%, respectively. The proposed method was implemented successfully for the simultaneous determination of PAR, PHE, and CPM in pharmaceutical formulations.
Chapter Three: includes the simple, rapid, and low-cost Q-absorption ratio method for simultaneous quantifying of PHE, CPM, and PAR in ternary mixtures without preseparation and using an advanced spectrophotometric method. For the resolving of the highly overlapped spectrum of the components of pharmaceutical formulations, the Q-absorption ratio and absorbance correction methods were selected. The method is based on measuring the absorbance at three different wavelengths of 296, 270, and 261 nm for the ternary mixture. Direct calculation of PAR was carried out at 296 nm while no interference was excited at this wavelength. After that, apply the absorbance correction method at 270 and 261 nm to remove the effect of PAR. Finally, the Q-absorption ratio approach was used to calculate the concentrations of PHE and CPM. The results showed that simultaneous determination of PAR, PHE, and CPM could be conducted within the range of 1–33 µg/mL, 1–23 µg/mL, and 1–36 µg/mL, respectively. The relative standard deviations for the simultaneous determination of PHE, CPM, and PAR were 0.89%, 1.02%, and 0.64%, respectively. Using the suggested method, PAR, PHE, and CPM were all found at the same time in pharmaceutical formulations.
Chapter Four: involves the derivative analytical methods for simultaneous quantification of PHE, CPM, and PAR as a ternary mixture in standard solutions and real sample solutions. The first method was the first-order derivative absorption of the ratio spectra developed by measurement at λmax of the drugs in the spectrum ratio of 14 µg/mL of PHE, CPM, and PAR mixture. PHE, CPM, and PAR showed the linear range for applying derivative ratio method in the series 0.1 – 30 µg/mL, 0.5 – 36 µg/mL, and 1 – 30 µg/mL, respectively. The relative standard deviation for the simultaneous determination of PHE, CPM, and PAR were 0.181%, 0.132%, and 0.141%, respectively. The second method was the second derivative method for the simultaneous determination of PHE, CPM, and PAR in their mixtures by following the zero-crossing principle, when one component has absorbance, the others were zero-cross. Select the wavelength determination for PHE, CPM, and PAR were 280.5 nm, 250.5 nm, and 245.5 nm, respectively. The range of the working in second derivative method were 3 – 24 µg/mL for PHE, 1 – 15 µg/mL for CPM, and 0.1 – 14 µg/mL for PAR. The percent relative standard deviation for PHE, CPM, and PAR in the proposed method were 1.96, 2.64, and 2.24, respectively. The approaches were found to be sensitive, accurate, and precise. For the simultaneous measurement of PHE, CPM, and PAR in laboratory generated mixes and tablets, planned techniques worked well. A better recovery percentage was found with low standard deviation for derivative ratio method compared to second derivative method. In conclusion, the suggested approaches were successful in simultaneously determining PAR, PHE, and CPM in pharmaceutical formulations.
Finally, the results of the simultaneous determination of PAR, PHE, and CPM in their tablets by the proposed methods were compared with the results of HPLC as the standard method for the PAR, PHE, and CPM in tablets, and the t-test and F-test between the proposed method and the standard method showed no significant difference between them.