Development and Validation of Analytical Methods for Quantification of Some Novel Drugs in Formulation.

Meena, M (2012) Development and Validation of Analytical Methods for Quantification of Some Novel Drugs in Formulation. Doctoral thesis, Vels College of Pharmacy, Chennai.


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Analytical chemistry is the study of separation, identification and quantification of the chemical components of natural and artificial material. Quantitative analysis gives an indication of identity and purity of the chemical species in the sample and quantitative analysis determines the amount of one or more of these components. The separation of components often performed prior to analysis. Analytical chemistry is also focused on improvement in experimental design, chemometrics and creation of new measurement tools to provide better chemical information. Analytical instrumentation plays an important role in production and evaluation of new product. Analytical technique is a method that is used to determine the concentration of a chemical compound or chemical element. There are a wide variety of techniques used for analysis, from simple weighing to titration to advanced techniques using highly specialized instruments. The most common techniques used in analytical chemistry are the following. • Titrimetry, based on the quantity of the titrant needed to react with the analyte. • Electroanalytical methods, includes potentiometry and volumetry. • Spectroscopy based on the differential interaction of the analyte along with electromagnetic radiation. • Chromatography in which the analyte is separated from the rest of the sample so that it may be measured without interference from other compounds • Microscopy • Bio-analysis • Radio analytical chemistry In present study simultaneous equation in UV methods, RP- HPLC and HPTLC were developed and validated for some of the selected formulations containing two drug combinations. UV spectroscopic methods solving simultaneous equation is developed and validated for the following drug combination and formulation i. Naproxen & Esomeprazole magnesium ii. Temisartan & Cilinidipine iii. Cilastatin sodium & Imipenem iv. Propranolol hydrochloride & Alprazolam In UV spectroscopy all the selected raw materials were dissolved in methanol and their spectra were recorded and the formulations were analysed. The actual amount of drugs in formulation was calculated by solving simultaneous equation. As the methods require only methanol as a solvent and less time consuming process, it can be followed in routine analysis to standardize the raw material as well as finished products with reproducible results. The following drug combinations & their formulations were estimated and validated by RP-HPLC. i. Naproxen & Esomeprazole magnesium ii. Telmisartan & Cilinidipine iii. Cilastatin sodium & Imipenem iv. Propranolol hydrochloride & Alprazolam v. Aspirin & Isosorbide mononitrate In RP-HPLC mobile phase and stationary phase played an important role in the resolution of the drugs. Chromatographic conditions were optimized before the development of chromatogram. Then the system suitability parameters were calculated. The formulations selected were then analyzed using fixed chromatographic parameters. The data obtained were subjected to statistical analysis. The developed RP-HPLC methods were validated for specificity, repeatability, reproducibility, linearity, robustness, stability of solution and system suitability as per ICH guidelines. As the methods are accurate, reproducible and highly sensitive at microgram levels of analyte it can be conveniently used in drug control laboratories and in industries to estimate the drug content in raw materials as well as in finished products. The following drug combinations and its formulations were estimated by HPTLC i. Naproxen & Esomeprazole magnesium ii. Telmisartan & Cilinidipine iii. Propranolol hydrochloride & Alprazolam iv. Aspirin & Isosorbide mononitrate In HPTLC technique system suitability parameters were fixed and the drug combination were injected, analysed. HPTLC method requires microgram levels of sample for its analysis. Simultaneous analytical procedure are now being used more frequently for estimation of drugs in multi component pharmaceutical formulations due to the following reasons i. Time consuming extraction and separations are avoided ii. Usage of expensive reagents has been minimized. From the above discussion, it was concluded that all UV spectrophotometric, RP-HPLC and HPTLC methods were found to be accurate, economic and rapid. Hence, the developed methods could be conveniently adopted for the routine analysis in formulations and for analyzing raw materials.

Item Type: Thesis (Doctoral)
Uncontrolled Keywords: Development; Validation; Analytical Methods; Quantification; Some Novel Drugs; Formulation
Subjects: PHARMACY > Pharmaceutical Chemistry
Depositing User: Subramani R
Date Deposited: 18 Jun 2017 08:11
Last Modified: 15 Oct 2022 02:41

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