Development and Validation of Various Instrumental Methods for the Estimation of Certain Selected Drugs in Formulations

Manjula Devi, A S (2012) Development and Validation of Various Instrumental Methods for the Estimation of Certain Selected Drugs in Formulations. Doctoral thesis, The Tamilnadu Dr.M.G.R. Medical University, Chennai.

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The UV spectrophotometric methods described in the present study were found to be rapid, reliable, and convenient for the quantification purpose of the selected antipsychotic drugs in single and combined dosage forms. These methods were very simple and required no pH adjustment and reagents. Improved spectral resolution was achieved, especially with the second order derivative spectroscopic methods. The results presented clearly demonstrated that the drugs in tablet dosage form can be determined by the UV-spectroscopic methods developed. Being simple, economic and direct methods of good accuracy and reproducibility, the proposed UV spectrophotometric methods can be recommended as good alternative methods for the routine quality control of the selected antipsychotic drugs in single and combined dosage forms when advanced instruments like HPLC are not available for routine quantification purpose. The validated spectrofluorimetric methods developed for the assay of zotepine, paliperidone and levosulpiride were found to be superior in sensitivity compared to other methods. The recommended procedures of paliperidone and levosulpiride have been effectively applied for the quantitative estimation of respective drugs in their pharmaceutical preparation. They can be considered as good alternatives to the high cost HPLC methods. The spectrofluorimetric methods can be further extended in biological fluids owing to their high sensitivity and selectivity. The described RP-HPLC methods for the quantitative estimation of selected antipsychotic drugs and combinations possessed several advantages such as highly acceptable resolution within a reasonable time using simple mobile phase system. The analytical results were reproducible, highly precise and accurate. The most critical system suitability parameters were carefully evaluated throughout the chromatographic analysis. The internal standards chosen in the current study have met all the necessary criteria. The retention time lower than 10 minutes grants speed to the routine analysis for all the selected drugs with better accuracy and selectivity. All the validation parameters were found to be within the acceptance criteria. The high correlation coefficient obtained from the linear regression analysis was indicative of the good linear relationship between concentration and responses. The RSD values lower than 2% in the validated techniques confirmed method precision. Mean recovery close to 100% demonstrated the accuracy of the methods. Robustness evaluation of the methods has shown fairly constant response over a variety of minor changes in the experimental conditions. The study also explored the application of RP-HPLC method for the in-vitro interaction studies by inferring about the displacement interactions of pimozide, a typical antipsychotic with commonly co-administered NSAIDs like aceclofenac, diclofenac sodium and lornoxicam. The main advantage of the RP-HPLC method described for the in-vitro drug displacement interaction study of pimozide was the applicability of the same chromatographic conditions for three different drug-drug interaction studies such as pimozideaceclofenac, pimozide-diclofenac and pimozide-lornoxicam. Statistical evaluation by F- test confirmed that there is significant difference in the amount of pimozide displaced by aceclofenac. In addition, the method was also effectively used for the quantitative estimation of pimozide in tablet formulation. The proposed HPTLC methods could provide highly selective quantitative stability indicating methods for zotepine, iloperidone, levosulpiride and pimozide in presence of their degradation products. It was observed that the degradants were well resolved from the analyte peaks. Under the optimized experimental conditions, the developed HPTLC methods for the simultaneous estimation of levosulpiride-rabeprazole, olanzapine-fluoxetine and trifluoperazinechlordiazepoxide enabled better sensitivity and a wider linear range. These characteristics demonstrate clear advantage over the previously reported methods. The performance of the methods was also found to be satisfactory when the analysis of commercial formulation was carried out. The method could minimize the cost of reagents and time of analysis. The various instrumental methods developed for the selected drugs in the current study have been well validated as per ICH recommendations. Validation of the described methods demonstrated excellent repeatability, specificity, accuracy and robustness. Excellent linearity of the calibration curves was proved by high values of correlation coefficients. The low values of RSD reflected the usefulness of the method in routine quality control purposes. The results of small variation in the experimental and instrumental parameters proved the reliability during normal use and suggested that the developed methods were robust. Statistical evaluations further strengthened the validity of all the methods developed. Favourable results were obtained when compared with the reported methods. Moreover, the current methods offer many advantages over the reported methods with respect to sensitivity as evidenced by the low LOD and LOQ values, wide range of linearity and the procedures were not as laborious as the reported methods. The results observed in the current study indicated that the newly developed methods can be classified as highly selective and sensitive. These developed methods can be successfully used for the routine quality control analysis of the selected antipsychotic drugs and combinations in bulk as well as formulations without interference from commonly encountered dosage form additives.

Item Type: Thesis (Doctoral)
Uncontrolled Keywords: Development and Validation, Various Instrumental Methods, Estimation of Certain Selected Drugs, Formulations.
Subjects: PHARMACY > Pharmaceutical Chemistry
Depositing User: Subramani R
Date Deposited: 11 Jan 2022 02:12
Last Modified: 11 Jan 2022 16:43

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