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