ich usfda validation differences
Post on 22-Jan-2018
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Represent by : Kushal shahMpharm (Ph. Analysis)
ICH/USFDA
VALIDATION PARAMETERSOF
ANALYTICAL METHOD
FDA-guidelines:◦ Validation is establishing documented evidence
which provides a high degree of assurance that a specific process will consistently produce a product meeting its pre-determined specifications and quality attributes
“Methods validation is the process of demonstrating that analytical procedures are suitable for their intended use”
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USP Specificity
Linearity and Range
Accuracy
Precision
Limit of Detection
Limit of Quantitation
Ruggedness
Robustness
ICH Specificity
Linearity
Range
Accuracy
Precision
◦ Repeatability
◦ Intermediate Precision
◦ Reproducibility
Limit of Detection
Limit of Quantitation
ICH takes system suitability as apart of the method validation,whereas the USP deals it in asepárate chapter.
Robustness for the ICH is part ofprecision.
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Ability of an analytical method to measure the analyte free from interference
due to other components.
Specificity
Ability to assess unequivocally the analyte in the presence of of components which
may be expected to be present (impurities,degradants, matrix)
Selectivity
describes the ability of an analytical method to differentiate various
substances in a sample
Original term used in USP
Also Preferred by IUPAC and AOAC
Also used to characterize chromatographic columns
Degree of Bias (Used in USP)
The difference in assay results between the two groups
- the sample containing added impurities, degradation products, related chemical compounds,
placebo ingredients
- the sample without added substances
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Ability of an assay toelicit a direct andproportionalresponse to changesin analyteconcentration.
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Closeness of the test results obtained by the method to the true value.
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The closeness of
agreement (degree of
scatter) between a
series of
measurements
obtained from multiple
samplings of the same
homogeneous sample.
Should be investigated
using homogeneous,
authentic samples.
◦ Precision…
Considered at 3 Levels
◦ Repeatability
◦ Intermediate Precision
◦ Reproducibility
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Precision under the same operating conditions over a short interval of time.
Method
- 9 determinations covering the specified range
- or: 6 determinations at 100% of the test concentration
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Definition: Ability reproduce data within the
predefined precision
Determination: SD, RSD interval
◦ Repeatability test at two different labs.
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LOD
Lowest amount of
analyte in a sample
that can be detected
but not necessarily
quantitated.
Estimated by Signal to
Noise Ratio of 3:1.
LOQ
Lowest amount of
analyte in a sample
that can be quantified
with suitable accuracy
and precision.
Estimated by Signal to
Noise Ratio of 10:1. 7/21/2016 10
Definition: Capacity to remain unaffected by
small but deliberate variations in method
parameters
Determination: Comparison results under
differing conditions with precision under normal
conditions
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Degree of reproducibility of test results under a
variety of conditions
Different Laboratories
Different Analysts
Different Instruments
Different Reagents
Different Days
Etc.
Expressed as %RSD
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Acceptable range having linearity, accuracy, precision.
For Drug Substance & Drug product Assay
◦ 80 to 120% of test Concentration
For Content Uniformity Assay
◦ 70 to 130% of test Concentration
For Dissolution Test Method
◦ +/- 20% over entire Specification Range
For Impurity Assays
◦ From Reporting Level to 120% of Impurity Specification for
Impurity Assays
◦ From Reporting Level to 120% of Assay Specification for
Impurity/Assay Methods
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Definition
◦ Set of parameters and criteria there off to ensure the system is working properly.
Aspects
- Dependent on type of test
- For chromatographic methods: tailing factor, rel.retention times, resolution factor, rel. st.deviation, number of theoretical plates
- To be checked before start of run and to beverified afterwards
- Described in Pharmacopoeias
System Suitability Test
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THANK YOU
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