This presentation include general introduction to validation of analytical method . analytical method validation include following points such as : Introduction Objective ,Types of analytical procedures to be validated,Validation parameters as per ICH and USP , cleaning validation , procedure , validation data, accuracy , range , precision, LOD, LOQ ,linearity, ruggedness , robustness

1. Analytical method validation as per
ICH and USP
Presented By –Vasanti G. Patil
M. Pharm First Yr.(QAT) 2020
Roll No. 26
Guided By – Dr. Sonali Mahaparale
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2. CONTENTS
 Introduction
 Objective
 Types of analytical procedures to be validated
 Validation parameters as per ICH and USP
 Conclusion
 Reference
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3. Introduction
Validation is the documented act of proving
that any procedure, process, equipment,
material, activity or system actually leads to
the expected result.
or
Analytical method validation is a process of
documenting/proving that an analytical method
provides analytical data acceptable for the
intended use.
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4.  The main objective of analytical validation is to
ensure that a selected analytical procedure will give
reproducible and reliable results that are adequate
for the intended purpose.
 This is applicable to all the procedure either
pharmacopoeial or non pharmacopoeial.
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5. Types of analytical procedures to be validated
 The required validation parameters also termed “ analytical performance
characteristics”, depends upon the type of analytical method.
 Pharmaceutical analytical methods are characterized into 5 general types
 Identification tests
 Potency assays
 Limit tests for the control of impurities
 Impurity tests- quantitative
 Specific tests
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6. Validation parameters as per ICH/USP
USP
 Specificity
 Linearity or range
 Accuracy
 Precision
 Limit of detection
 Limit of quantitation
 Ruggedness
 Robustness
ICH
 Specificity
 Linearity
 Range
 Accuracy
 Precision
 Limit of detection
 Limit of quantitation
 Robustness 624-01-2020

7. Accuracy
“The accuracy of an analytical procedure is the closeness of agreement
between the values that are accepted either as conventional true values or an
accepted reference value and the value found”.
Determination
Assay
i. Drug substance
ii. Drug product
iii. Impurities (quantitation)
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8. Recommended data:
Assessed by 9 determinations over a minimum of 3 concentration levels
covering a specified range.
Limit
Typical accuracy of the recovery of the drug substance is expected to be about
99 – 101%.
Typical accuracy of the recovery of the drug product is expected to be about
98 – 102%.
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9. Precision
“The closeness of agreement (degree of scatter) between a series of
measurements obtained from multiple samplings of the same homogeneous
sample”.
 Precision includes:
 Repeatability
 Intermediate Precision
 Reproducibility
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10. Repeatability
• Repeatability expresses the precision under the same operating conditions over
a short interval of time.
• Repeatability should be assessed using a minimum of 9 determinations
covering the specified range.
Intermediate precision
• Intermediate precision expresses variations within laboratories, such as
different days, different analysts, different equipment etc.
Reproducibility
• Reproducibility expresses the precision between laboratories.1024-01-2020

11. Following parameters should be reported
a. Standard deviation.
b. Relative standard deviation.
Concentration
µg/ml
Absorbance SD and %RSD
8
0.337
0.334
0.341
0.00041
1.223%
12 0.575
0.583
0.596
0.0106
1.158%
20 0.967
0.985
0.978
0.0091
0.993%
0
0.2
0.4
0.6
0.8
1
1.2
8 12 20
Absorbance
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13. LOD and LOQ
 The limit of detection (LOD) is
usually defined as the lowest
quantity or concentration of a
component that can be reliably
detected with a given analytical
method.
 LOQ are terms used to describe
the smallest concentration of an
analyte that can be reliably
measured by an analytical
procedure
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14. Determination of LOD and LOQ
Limit of detection Method
 Based on visual examination.
 Based on standard deviation of response and slope.
 Signal to noise ratio 2:1 or 3:1
Limit of quantitation Method
 Based on visual examination.
 Based on standard deviation of response and slope.
 Signal to noise ratio 1424-01-2020

15. Specificity
Specificity is the ability to assess
unequivocally the analyte in presence of
components which may be expected to be
present.
Determination
• Identification tests
• Assay and impurity test(s)
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16. Linearity
 The Ability of the method to obtain test results that are directly
proportional to concentration within a given range.
 Method: dilution of stock solution/separate weightings
 Minimum 5 concentrations are used
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17. Range
 The interval between the upper and lower concentrations of analyte in the
sample that have been demonstrate to have a suitable level of precision,
accuracy, and linearity.
 Specific range dependent upon intended application of the procedure.
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18. Range(Continued)
 Assay: 80 to 120% of test concentration.
 Content uniformity: 70 to 130% of test concentration.
 Dissolution: 20% to 120%
 Impurities reporting level: 120% of specification limit (with respect to test
concentration of API)
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19. Ruggedness
 The ruggedness of an analytical method is the degree of reproducibility of
test results obtained by the analysis of the same samples under a variety of
conditions, such as different laboratories, different analysts, different
instruments, different days, etc.
Certain may include
• Source
• Concentration and stability of solution
• Heating rate
• Column temperature
• Humidity 1924-01-2020

20. Robustness
“The robustness of an analytical procedure is a measure of its capacity to
remain unaffected by small, but deliberate variations in method parameters
and provides an indication of its reliability during normal usage”.
Determination:
The evaluation of robustness should be considered during the development
phase and depends on the type of procedure under study.
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21. System suitability
 System suitability testing is an integral part of many analytical
procedures.
 The tests are based on the concept that the equipment, electronics,
analytical operations and samples to be analyzed constitute an integral
system that can be evaluated as such.
 System suitability testing has been recommended by USP in HPLC
procedures. 2124-01-2020

22. Conclusion
 When the method is properly validated consistent, reliable and
accurate results are obtained.
 Analytical method validation is an important analytical tool to ensure
the accuracy and specificity of the analytical procedures with a
precise agreement.
 Validation of analytical methods is also required by regulations.
 Hence it is very important to validate any analytical method that has
been developed
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24. References
1.Gupta P. C method validation of analytical procedures. pharmatutor. 2015;3(1):32-39.
2. Lopez P, Buffoni E, Pereira F, Vilchez Quero J. Analytical Method Validation. Wide
Spectra of Quality Control. 2011;:1-19.
3. [Internet]. Who.int. 2016 [cited 2 March 2019].
https://www.who.int/medicines/areas/quality_safety/quality_assurance/Guideline_Validation
_AnalyticalMethodValidationQAS16-671.pdf
4. Daksh S. VALIDATION OF ANALYTICAL METHODS – STRATEGIES &
SINGFICANCE. International Journal of Research and Development in Pharmacy and Life
Sciences. 2015;4(3):1489-1497. 2424-01-2020

25. Thank You
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