It was one of my presentation for my master's in pharmacy. It assisted me in better understanding the many pharmacy research fields as well as what to do before, during, and following a research project. I am hoping that it will also provide the readers a better understanding of the fascinating world of research.

1. Research Trends in Different Pharmaceutical Areas:
Analytical Method Development

2. Name
Md.
Nazmul
Islam

3. Analytical Method Development
It is the process of selecting an accurate assay procedure to
determine the composition of a formulation.
Proving an analytical method that is acceptable for use in
laboratory to measure the concentration of samples.

4. Analytical methods should be used within
GMP and GLP environments and must be
developed using the protocols and
acceptance criteria set out in the ICH
guidelines Q2(R1)
Analytical Method Development

5. The prerequisite for method development:
Qualified
and calibrated
instruments
Documented
methods
Qualified
analysts
Reliable
reference
standards
Change
control
Analytical Method Development

6. An analytical method details the steps and techniques necessary to
perform an analysis.
Preparation of
samples,
standards and
reagents
Use of
apparatus
Generation of
the
calibration
curve
Use of the
formula for
the
calculation
This may
include
Analytical Method Development

7. Steps for Analytical Method Development
Purpose
Highlighting of
Steps
Characterization of
the Analyte
Requirements
Review of
Literature and
Previous Methods
Choosing an
Analytical Method
Setting up of
Instruments
Optimization of
the Method
Analytical Figures
of Merit
Documentation
Development
Method
Evaluation
Sample
Estimation

8. Category of Analytical Method and Method Development
• quantitation
of active
ingredients
Category
• determination
of impurities
Category
• determination
of
performance
characteristic
s
Category
• identification
tests
Category

9. Life Cycle of Analytical Method Development
Procedure Design
(development and
understanding)
Procedure
performance
qualification
Procedure
performance
verification

10. Development of method
Validation of the method
Method in routine use
Change the method
Validated yet
unchanged
Revalidation
needed due to
change
Redevelopment
required due to
change
Validated and
reformed

11. Content of Analytical Procedures
Principle
Apparatus
Operating
Parameters
Standards
Sample
Preparation
Procedure
System
Suitability
Calculations
Data
Reporting

12. Method validation is a procedure of performing
numerous assessments designed to verify that an
analytical test system is suitable for its intended reason
and is capable of providing beneficial and legitimate
analytical data.
Method Validation

13. Importance of Analytical Method Validation
Ensuring quality of the product
For acceptance of the products
For registration of any pharmaceutical
product or pesticide formulation
For proficiency testing

14. Types of Analytical Method to be Validated
Types
•Identification
tests
•Quantitative
tests for active
moiety
•Limit tests
•Quantitative
tests for
impurities

15. Characterization of Method Validation
Accuracy
Precision
Linearity
Range
LOD
LOQ
Selectivity
Robustness
System
suitability
studies

16. Content Uniformity
50% to 150 % of the test
concentration from the
lower strength
U.S. FDA Guidelines for Analytical Method Validation
Assay
50 to 150 % of the test
concentration
correlation
coefficient
should obtain
≥ 0.999

17. Dissolution
50 to 150 % of the test
concentration. If sustained
product 10% to 150 % of the
test concentration
U.S. FDA Guidelines for Analytical Method Validation
Uniformity of
Dosage Units
50% form the lower strength
and to 150 % of the test
concentration from the
higher strength (if different
strengths are available)
correlation
coefficient
should obtain
≥ 0.999

18. When Analytical Methods Need to be Validated
Before initial use in routine testing
When transferred to another laboratory

19. Usefulness of Analytical Method Development
New process
and reactions New molecule
development
Achieving
acceptance of
products by the
international
agencies
Assuring quality

20. Usefulness of Analytical Method Development
Impurity
profiling Degradation
studies
Mandatory
requirement
purposes for
accreditation as
per ISO 17025
guidelines

21. Challenges in Analytical Method Development
More attention should be paid to the development of these
new methods
The development timelines are compressed for various
reasons
Once an analytical method is approved, there is usually
great resistance to submit changes to FDA
The analytical methods need to be validated for any GMP
activities

22. Advantages of Analytical Method Development
Reduces the time and costs of analysis
Increases accuracy and precision of analysis
Ensures the identity, purity, safety, efficacy and performance of
drug products
Helps drug approval by regulatory authorities

23. Analytical Techniques used in Analytical Method Development
Chromatographic
Methods
Spectroscopic
Techniques
Photometric
Methodology
Electrochemical
Technique
Electrophoretic
Technique
Hyphenated
Techniques

24. Chromatographic Methods
It is a common technique
for analyzing a wide
range of organic and
inorganic compounds
 Thin-Layer Chromatography

25. Chromatographic Methods
It is used to separate
complicated mixtures of
molecules found in
chemical and biological
systems
 High Performance Liquid Chromatography

26. Chromatographic Methods
It is a potent separation
technique for detecting
volatile organic
molecules
 Gas chromatography

27. Spectroscopic Method

28. References
 Chauhan A, Mittu B, Chauhan P. Analytical method development and
validation: a concise review. Journal of Analytical & Bioanalytical Techniques.
2015; 06(01): 1-5. DOI: 10.4172/2155-9872.1000233
 Ravichandran V, Shalini S, Sundram KM, Rajak,H. Validation of analytical
methods-strategies & importance. International Journal of Pharmacy and
Pharmaceutical Sciences. 2010; 2(3): 1822.
 Sharma S, Singh N, Ankalgi AD, Rana A, Ashawat MS. Modern trends in
analytical techniques for method development and validation of
pharmaceuticals: a review. Journal of Drug Delivery and Therapeutics. 2021;
11(1-s): 121-130. DOI: 10.22270/jddt.v11i1-s.4515

29. References
 Ravisankar P, Navya CN, Pravallika D, Sri DN. A review on step-by-step
analytical method validation. IOSR Journal of Pharmacy. 2015; 5(10): 07-19.
 Lubrizol Life Science. Analytical method development and validation
[Internet]. Bethlehem PA: Lubrizol Life Science; 2019 [updated 2019 Nov 27;
cited 2022 Mar 19]. Available from: https://lubrizolcdmo.com/technical-
briefs/analytical-method-development-and-validation/
 Beckett AH, Stenlake JB, editors. Chromatography. In: Practical Pharmaceutical
Chemistry (4th Ed, Part II). New Delhi: CBS Publishers and Distributors; 2004:
85-174