A number of new drug entities, modifications of existing ones, and multi-component formulations are entering the market, every year. Development of simple analytical methods for analysis of various drugs in multi - component formulations is a tricky task for an analytical researcher. As analytical techniques are used throughout drug development, manufacturing, release of drug products, the reliability of their results is essential. Chromatographic methods are most useful and powerful techniques for qualitative and quantitative determination of drug/s. Therefore, appropriate validation to demonstrate the performance and suitability of the analytical method is much more than a formal requirement. Hence, there is need to develop and validate correct analytical method for these medicine/s.
This book details,
- Development and validation of HPTLC - densitometric method for concurrent estimation of metformin hydrochloride, pioglitazone hydrochloride and gliclazide in combined dosage form.
- Development and validation of HPTLC method for simultaneous estimation of moxifloxacin hydrochloride and dexamethasone sodium phosphate in combined pharmaceutical dosage form.
- Development and validation of RP - HPLC method for simultaneous estimation of ciprofloxacin hydrochloride and dexamethasone in combined dosage form, which is better alternative to existing one.
The developed analytical methods are simple, selective, accurate, robust, and precise with shorter analysis time for the analysis of drug/s in combined pharmaceutical dosage forms. All the developed HPTLC and HPLC methods have been validated as per ICH Q2 (R1) guidelines. Developed analytical methods could boost analytical researcher to work more efficiently in the field of analytical method development and validation of Pharmaceutical dosage forms.
Table of Contents
1. Introduction
2. Drug Profile
3. Aims and Objectives
4. Plan of Work
5. Results and Discussion
6. Experimental
7. References
Research Objectives and Focus
This work aims to address the challenges in the quality control of multi-component pharmaceutical formulations by developing and validating simple, accurate, and robust chromatographic methods, specifically utilizing High-Performance Thin-Layer Chromatography (HPTLC) and Reverse-Phase High-Performance Liquid Chromatography (RP-HPLC) in accordance with ICH Q2 (R1) guidelines.
- Development of HPTLC methods for the simultaneous estimation of Metformin, Pioglitazone, and Gliclazide.
- Development of HPTLC methods for the simultaneous estimation of Moxifloxacin and Dexamethasone sodium phosphate.
- Development of an improved RP-HPLC method for the simultaneous estimation of Ciprofloxacin and Dexamethasone.
- Application of these validated analytical methods to determine drug content in commercially available marketed formulations.
Excerpt from the Book
Selection of mobile phase:
Aliquot portions of standard drug solutions were applied on silica gel TLC plates and used for selection of mobile phase. Based on the literature survey26 toluene: ethyl acetate: methanol: ammonia (2: 7: 3: 0.2, v/v/v/v) was used as initial mobile phase, but there was little movement of MOXI and no movement of DEXA Na P. After that, different ratios of same components were used but DEXA Na P was not moving at all. Formic acid and acetic acid were also tried by replacing ammonia in the above mentioned solvent system, but results showed a very broad peak for DEXA Na P. After that, different solvents with varying polarity as well as combination of solvents were tried based on the literature to get well resolved bands of the drugs. After trying several permutations and combinations, the solvent system containing dichloromethane: methanol: ammonia: acetonitrile in the ratio of (6: 5: 2.5: 5, v/v/v/v) was found to be most satisfactory as it gave good resolution for both the drugs. Hence, the same was used for all further studies of this combination of drugs.
Summary of Chapters
Introduction: Provides a comprehensive overview of analytical chemistry, the classification of various analytical methods, and the fundamental principles of UV-Visible spectroscopy and chromatography.
Drug Profile: Presents detailed chemical structures, properties, and therapeutic categories for the pharmaceutical compounds investigated in this study.
Aims and Objectives: Outlines the necessity for new, validated analytical methods and defines the specific research goals regarding the simultaneous estimation of selected drug combinations.
Plan of Work: Details the systematic research strategy, including the selection of techniques and the procedural steps for method development and validation.
Results and Discussion: Discusses the optimization of chromatographic conditions, validation parameters such as linearity, precision, and accuracy, and the application of these methods to market samples.
Experimental: Describes the materials, instruments, software, and methodological procedures used to conduct the experimental research.
References: Lists the academic and technical sources utilized to support the methodology and findings of the research.
Keywords
Analytical Chemistry, Chromatography, HPTLC, RP-HPLC, Method Validation, Simultaneous Estimation, Metformin, Pioglitazone, Gliclazide, Moxifloxacin, Dexamethasone, Ciprofloxacin, Quality Control, Pharmaceutical Formulations, ICH Guidelines
Frequently Asked Questions
What is the primary focus of this research?
The research focuses on the development and validation of reliable, chromatographic analytical methods (HPTLC and HPLC) for the simultaneous estimation of various multi-component drug formulations to ensure quality control.
What are the central thematic areas of the book?
The central themes include the design of separation methods, optimization of chromatographic conditions, adherence to ICH guidelines for method validation, and the practical application of these methods to commercial pharmaceutical products.
What is the ultimate goal of the work?
The primary goal is to provide accurate, precise, and robust analytical procedures that allow for the efficient simultaneous analysis of multi-component drug combinations that are not currently well-addressed by existing pharmacopoeial methods.
Which scientific methods are primarily utilized?
The study primarily utilizes High-Performance Thin-Layer Chromatography (HPTLC) and Reverse-Phase High-Performance Liquid Chromatography (RP-HPLC).
What does the main body of the work cover?
The main body covers the theoretical background of chromatography and spectroscopy, specific method development for three distinct drug combinations, comprehensive validation studies (linearity, precision, accuracy, specificity, robustness), and practical application to marketed eye drop and tablet formulations.
How is the validation of the methods demonstrated?
Validation is demonstrated through rigorous testing according to ICH Q2 (R1) guidelines, specifically measuring parameters like accuracy, precision (repeatability and intermediate precision), specificity, limit of detection, and limit of quantification.
Why is HPTLC often preferred in this study for certain combinations?
HPTLC is highlighted for its advantages such as short development time, a wide choice of stationary phases, and the ability to visualize separated compounds, making it a powerful tool for complex pharmaceutical mixture analysis.
How is the suitability of the chromatographic system determined?
Suitability is determined by evaluating system suitability parameters such as resolution (Rs), capacity factor (k), selectivity factor (α), number of theoretical plates (N), and tailing factor (T).
- Arbeit zitieren
- Dr. Satish Gabhe (Autor:in), Dr. Kakasaheb Mahadik (Autor:in), Sachin Potawale (Autor:in), Anirudh Thati (Autor:in), 2013, Simultaneous Estimation of Some Drugs in Bulk and in their Formulation by Chromatographic Methods., München, GRIN Verlag, https://www.grin.com/document/272088
