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    Analytical Method Validation Checklist

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    Sangram Kendre
    The document provides checklists for validation of analytical methods for assay/related substances and dissolution testing of chemical parameters. The checklists include common validation parameters such as specificity, linearity, range, accuracy, precision (repeatability and intermediate precision), detection limit, quantitation limit, and system suitability testing. Acceptance criteria for each parameter are also defined.

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    © All Rights Reserved
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    Analytical Method Validation Checklist

    Uploaded by

    Sangram Kendre
    401 views5 pages
    The document provides checklists for validation of analytical methods for assay/related substances and dissolution testing of chemical parameters. The checklists include common validation parameters such as specificity, linearity, range, accuracy, precision (repeatability and intermediate precision), detection limit, quantitation limit, and system suitability testing. Acceptance criteria for each parameter are also defined.

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    The document provides checklists for validation of analytical methods for assay/related substances and dissolution testing of chemical parameters. The checklists include common validation parameters such as specificity, linearity, range, accuracy, precision (repeatability and intermediate precision), detection limit, quantitation limit, and system suitability testing. Acceptance criteria for each parameter are also defined.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    401 views5 pages

    Analytical Method Validation Checklist

    Uploaded by

    Sangram Kendre
    The document provides checklists for validation of analytical methods for assay/related substances and dissolution testing of chemical parameters. The checklists include common validation parameters such as specificity, linearity, range, accuracy, precision (repeatability and intermediate precision), detection limit, quantitation limit, and system suitability testing. Acceptance criteria for each parameter are also defined.

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    Checklist for Analytical Method Validation (Chemical)

    TEST ASSAY/RELATED SUBSTANCES


    PARAMETER No. DOCUMENTS REQUIRED AVAILABILITY
    1 Testing Method
    2 Acceptance criteria
    3 Chromatogram/spectrum for following solutions:-
    a) Standard
    b) Sample
    c) Blank/Placebo
    d) Spike solution
    e) System suitability tests
    4 Impurities available
    Specificity
    a) Peak purity for PDA detector or spike solution for non-PDA
    detector
    b) Relative Retention Time (RRT)
    c) Resolution (R) where applicable
    5 Impurities not available
    a) Stress data (minimum data for humidity, heat and light)
    b) Peak purity
    c) Relative Retention Time (RRT)
    d) Resolution (R) where applicable
    1 Testing Method
    2 Acceptance criteria
    Linearity 3 Minimum five (5) levels of standard solutions
    4 Data for linear regression equation, Y-intercept, slope, r2 and
    linearity graph
    1 For the assay of drug substances: 80% - 120% of working
    concentration (WC)
    Range
    2 For the determination of an impurity: from the reporting level of an
    impurity to 120% of the specification
    1 Testing Method
    2 Acceptance criteria
    3 Minimum three (3) levels of concentration in triplicates covering the
    specified range
    Accuracy
    4 Result : reported as percent recovery by the assay of known added
    amount of analyte in the sample, OR as the difference between the
    mean and the accepted true value together with the confidence
    intervals
    1 Testing Method (using sample/product as the test solution)
    Precision 2 Acceptance criteria
    (Repeatability) 3 Minimum three (3) levels of concentration in triplicates covering the
    specified range , OR
    minimum six (6) replicates at 100% of the WC
    4 Result : SD, RSD and confidence Interval
    1 Testing Method (using sample/product as the test solution)
    2 Acceptance criteria
    Precision 3 Minimum three (3) levels of concentration in triplicates covering the
    (intermediate specified range , OR
    precision/ minimum six (6) replicates at 100% of the WC
    ruggedness) 4 Cover at least 2 parameters among variation of analyst, date and
    equipment
    5 Result : SD, RSD and confidence Interval
    Detection Limit 1 Testing Method : visual observation / signal-to-noise / standard
    deviation of the response and the slope
    2 If based on standard deviation of the response and the slope
    method
    a) Minimum five (5) levels of standard solutions
    b) Peak area values for all concentrations
    c) Data for linear regression equation, Y-intercept, slope, r2 and
    linearity graph.
    3 Calculation/formulation where applicable
    4 Related Chromatogram(s) at LOD
    5 Value of detection limit
    Quantitation 1 Testing Method : visual observation / signal-to-noise / standard
    Limit deviation of the response and the slope
    2 if based on visual observation method, accuracy and precision data
    at LOQ must be provided
    3 If based on calibration curve method
    a) Minimum five (5) levels of standard solutions
    b) Peak area values for all concentrations
    c) Data for linear regression equation, Y-intercept, slope, r2 and
    linearity graph.
    5 Calculation/formulation where applicable
    6 Value of quantitation limit
    System 1 RSD, tailing factor, theoretical plate
    Suitability 2 Resolution (if two or more components)
    Testing
    Robustness 1 Testing Method
    (not mandatory) 2 Acceptance criteria
    3 Result : refer acceptance criteria for accuracy and precision
    (repeatability)
    Table A: Checklist for Assay/Related Substances
    TEST DISSOLUTION
    PARAMETER No. DOCUMENTS REQUIRED AVAILABILIT
    Y
    1 Testing Method
    2 Acceptance criteria
    3 Chromatogram/spectrum for following solutions:-
    f) Standard
    Specificity
    g) Sample
    h) Blank/Placebo
    i) Spike solution
    j) System suitability tests
    1 Testing Method
    2 Acceptance criteria
    Linearity 3 Minimum five (5) levels of standard solutions
    4 Data for linear regression equation, Y-intercept, slope, r2 and linearity
    graph.
    1 Dissolution testing: ± 20% over the specified range
    Example 1: if the specification is NLT 75% (Q) of the labelled amount is
    dissolved in 45 minutes, the validated range would be 60 – 100% of
    Range the label claim
    Example 2: if the specification for a controlled released product cover
    a region from 20% after 1 hour, up to 90%, after 24 hours, the
    validated range would be 0 – 110% of the label claim
    1 Testing Method
    2 Acceptance criteria
    3 Minimum three (3) levels of concentration in triplicates covering the
    specified range
    Accuracy
    4 Result : reported as percent recovery by the assay of known added
    amount of analyte in the sample, OR as the difference between the
    mean and the accepted true value together with the confidence
    intervals
    1 Testing Method (using sample/product as the test solution)
    2 Acceptance criteria
    Precision
    3 Minimum three (3) levels of concentration in triplicates covering the
    (Repeatability)
    specified range , OR minimum six (6) replicates at 100% of the WC
    4 Result : SD, RSD and confidence Interval
    1 Testing Method (using sample/product as the test solution)
    Precision
    2 Acceptance criteria
    (intermediate
    3 Minimum three (3) levels of concentration in triplicates covering the
    precision/
    specified range , OR minimum six (6) replicates at 100% of the WC
    ruggedness)
    4 Cover at least 2 parameters among variation of analyst, date and
    equipment
    5 Result : SD, RSD and confidence Interval
    System 1 RSD, tailing factor, theoretical plate
    Suitability 2 Resolution (if two or more components)
    Testing
    Robustness 1 Testing Method
    (Not Mandatory) 2 Acceptance criteria
    3 Result : refer acceptance criteria for accuracy and precision
    (repeatability)
    Table B: Checklist for Dissolution

    Note:
    1. The following validation parameters are required for COMPENDIAL METHOD (assay/related
    substances/dissolution):
    a) Specificity
    b) Precision (intermediate precision)
    c) System Suitability tests
    2. Please arrange the documents in sequence according to the checklist provided.
    Commonly Acceptance Criteria
    PARAMETER ACCEPTANCE CRITERIA
    Absence of interfering peaks in the placebo, impurity demonstrate specificity
    Specificity
    Pass peak purity test (particularly for related substances test)
    r2  0.995
    Linearity
    y-intercept at 100% working concentration ≤ 2%
    Measured recovery within 95% - 105%
    Accuracy or
    mean difference ± 2% & CI
    Precision RSD ≤ 2.0% & CI
    (Repeatability)
    Precision RSD ≤ 2.0% & CI
    (intermediate or
    precision/ mean difference ± 2% & CI
    ruggedness)
    Detection Limit LOD peak must be visible
    If based on standard deviation of the response and the slope method, DL = 3.3 Ó/S
    If based on signal to noise, S/N= 3:1 or 2:1
    Quantitation if based on visual observation method, accuracy and precision data at LOQ must be ± 20%
    Limit If based on standard deviation of the response and the slope method, DL = 10 Ó/S
    If based on signal to noise, S/N= 3:1 or 2:1
    System RSD ≤ 2%
    Suitability Theoretical plate/column efficiency, N ≥ 2000
    Testing Tailing factor < 2
    Resolution > 2
    Robustness Refer acceptance criteria for accuracy and precision (repeatability)
    (not mandatory)

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