Validation of Analytical Methods

Introduction
The concept of validation was first proposed by Food and Drug Administration (FDA)
official, Ted Byers and Bud Loftus in the mid-1970s in order to improve the quality of
Pharmaceutical.

1. Validation:

“Establishing documented evidence that provides high degree of

assurance that a specific process will consistently produce a product
meeting its pre-determined specifications and quality attributes.
This maintain and assure a higher degree of quality of food and drug
products

2. Need for validation:

Customer satisfaction, Customer mandated, product liability, control
product cost, the development of the next generation, safety.

3. Document of validation:
The validation activity cannot be completed without proper
documentation of each and every minute activity with utmost
details.
Document of validation generally different types
Such as
 VMP (validation master plan)
 VP (validation protocol)
 VR (validation reports)
 SOP (standard operating procedure)
 Validation of Analytical Methods
4. Types of validation:
 Process validation
 Cleaning validation
 Equipment validation
 Validation of analytical methods

TYPES OF PROCEDURE TO VALIDATION PROCEDURE

Parameters to be checked for method validation.
1. Selectivity/Specificity
The ability to assess the analyte when in the presence of
other components
2. Precision
A measure of the agreement for multiple measurements on
the same sample
3. Accuracy
An assessment of the different between the measured value
and true value
4. Linearity & Range
The proportionality and measurement of concentration
range
5. LOD & LOQ
The lowest amounts of analyte that can be detected/
determined accurately, respectively
6. Robustness
A check of the effect of deliberate small changes to the
method on the results
 Validation of Analytical Methods
Parameter Tests(examples)

Specificity Prove with specific method: HPLC, DAD,MS,dif

columns
Precision
Repeatability Minimum of 9determinations over the specified
Intermediate range
Reproducibility Over 3days, 2 operators, 2 instruments,
Only required testing is done indifferent laboratories

LOD Visual approach, S/N >=3

LOQ S/N>=10, Standard deviation of response

Linearity Min 5 concentrations : visual, correlation coefficient

Range 80 to 120% of test concentration , from linearity

tests

5.Conclusion
Validation has been proven assurance for the process efficiency
and sturdiness and its full-fledged quality attributing tool for the
pharmaceutical industries
Validation common word in the areas of drug development,
manufacture & specifications of finished products.

Presented by
Mr. VIGNYAN MACHIDI
Validation of Analytical Methods