Cleaning Validation - Comparative Analysis by saj38576

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									                                                                                                     TEM-020
                                                                                                     Issue date
                        Cleaning Validation – Comparative Analysis
                                                  (Ref.VAL-020)


     Project number:


     Protocol Number:


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COMAPARATIVE ANALYSIS
1.   Test Description
     This test is to be conducted to document the validation of a TOC analysis method for use in measuring
     samples for cleaning validation. A parallel analysis of samples will be carried out and compared using TOC
     and HPLC analysis.
2.   Test Objective
     To determine the linearity and precision of a series of standards measured by TOC and HPLC over a
     known concentration range.
          • To determine the accuracy and recovery of a series of standards measured by TOC and HPLC
            over a known concentration range.
          • To determine the limit of quantitation and limit of detection of a series of standards measured by
            TOC and HPLC over a known concentration range.
3.   Acceptance Criteria
      Test Objective            Measured Response                  Acceptance Criteria
      3.1. Linearity            The correlation coefficient        3.1.1. HPLC: equal to or greater than 0.997
                                  2
                                (R )    for     the  linear        3.1.2. TOC: equal to or greater than 0.980
                                concentration range.
      3.2. Accuracy             % recovery of the theoretical      3.2.1. HPLC: 90-110%
                                amount at all concentrations       3.2.2. TOC: 85-115%
                                tested.
      3.3. Limit           of   % RSD and % recovery               3.3.1. HPLC: lowest concentration of the “active”
            Quantitation                                           residue at which: The area %RSD of six replicate
                                                                   injections is less than or equal to 10 and recovery
                                                                   between 90-110% of the theoretical amount.
                                                                   3.3.2. TOC: lowest concentration at which: the
                                                                   area % RSD from four replicate injections is less
                                                                   than or equal to 15.0% and recovery of the
                                                                   “active” residue must be between 85-115% of the
                                                                   theoretical amount.
      3.4. Limit           of   Lowest detectable standard         3.4.1. HPLC: The lowest concentration of active
            Detection           concentration.                     residue that can be consistently detected for four
                                                                   consecutive replicate injections.
                                                                   3.4.2. TOC:
                                                                   • The lowest concentration of “active” residue
                                                                      that can be readily detected by the instrument
                                                                      in four consecutive injections.
                                                                   • The determined LOD must be equal to or
                                                                      greater than that carbon concentration obtained
                                                                      by multiplying the standard deviation of six
                                                                      injections of Type I water (18 megohms-cm
     File Location:                                Date Printed:                                  Page 1 of 4
                                                                                            TEM-020
                                                                                            Issue date
                      Cleaning Validation – Comparative Analysis
                                               (Ref.VAL-020)

      Actual   Active    Measured         Measured     Measured     Average      Mean %       % RSD
      Concentration      response 1       response 2   response 3   result       recovery
      (50%)
      (100%)
      (200%)
      (400%)
          Compare and summarise results according to acceptance criteria.
          3.2.2. TOC Analysis
      Actual    Total    Measured         Measured     Measured     Average      Mean %       % RSD
      Organic Carbon     TOC      1       TOC      2   TOC      3   TOC          recovery
      Concentration      (ppm)            (ppm)        (ppm)        (ppm)
      (ppm)
      (10%)
      (50%)
      (100%)
      (200%)
      (400%)
          Compare and summarise results according to acceptance criteria.
     3.3. Limit of Quantitation
          Determine Limit of Quantitation by assessing results of Accuracy test in accordance with the
          acceptance criteria for HPLC and TOC analysis and summarise the results.
          3.3.1. Limit of Quantitation for HPLC
          Document the LOQ concentration for HPLC analysis and how this was established.
          3.3.2. Limit of Quantitation for TOC
          Document the LOQ concentration for TOC analysis and how this was established.
     3.4. Limit of Detection
          Determine Limit of Detection by assessing results of Accuracy test in accordance with the acceptance
          criteria for HPLC and TOC analysis and summarise the results.
          3.4.1. Limit of Detection for HPLC
          Document the LOD concentration for HPLC analysis and how this was established.
          3.4.2. Limit of Detection for TOC
          Document the LOD concentration for TOC analysis and how this was established.


6.   Comments




7.   Conclusion




8.   Attachments
     Validation Discrepancy Forms - nil




     File Location:                             Date Printed:                             Page 3 of 4

								
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