- Specificity
- Linearity
- Accuracy
- Precision
- Assessing selected analytical performance characteristics to generate appropriate, relevant data rather than repeating the validation process.
- Method verification consists of partial validation. It should be performed for already validated analytical methods under the following circumstances:
- when an already validated method is used on a product for the first time (e.g. in case of a change in active pharmaceutical ingredient (API) supplier, change in the method of synthesis or after reformulation of a drug product).
- when an already validated method is used for the first time in a laboratory (in some cases, method transfer may be preferable).
- This document established the method selection & procedures for verification of standard method performance. The laboratory shall confirm that it can properly operate standard methods before introducing the tests or calibrations. If the standard method changes, the verification shall be repeated.
- Verification that a laboratory can adequately operate a standard method requires that the laboratory provide objective evidence the performance parameters specified in the test method have been met with the matrices to which the method is being applied. Most often, the critical requirements are the accuracy and the precision (generally accepted as repeatability and reproducibility) which are reflected in the measurement uncertainty. The objective evidence is the accuracy and precision obtained from actual lab data.
- The scope of verification of the analytical procedure for Accuracy, Precision, Specificity & Linearity is to demonstrate that the method is suitable for the analysis of Azithromycin Tablets USP 500 mg.
Equipments |
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HPLC |
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Instrument
ID & Calibration Date |
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Analytical
Balance |
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An
analytical balance sufficiently sensitive to detect changes of 0.1 mg. |
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Instrument
ID & Calibration Date |
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pH
Meter |
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Instrument
ID & Calibration Date |
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Chemicals |
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Methanol (HPLC Grade) |
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Acetonitrile (HPLC Grade) |
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Dipotassium Hydrogen Orthophosphate |
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Sodium 1 - Octane Sulfonate |
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Monobasic Ammonium Phosphate |
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Glassware |
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Volumetric Flasks |
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Pipettes |
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Beakers |
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Other Glassware |
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Documents |
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Standard Operating Procedure |
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Calibration Documents |
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Guidelines |
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(1226) Verification of Compendial
Procedures |
Working
Standard Used |
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Azithromycin Dihydrate USP |
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Reference No. |
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LOD |
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Purity (as is basis) |
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Prepared on |
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Valid up to |
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Sample
Taken for Verification |
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Name of Sample |
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Azithromycin Tablets USP 500
mg |
Batch Number |
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Manufacturing Date |
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Expiry Date |
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- System precision: To check system suitability criteria
- Repeatability should be assessed using a minimum of nine determinations covering the specified range for the procedure, e.g. three concentrations/three replicates each, or a minimum of six determinations at 100% of the test concentration.
- Intermediate precision expresses within laboratory variations (usually on different days, different analysts and different equipment).
Serial Number |
Sample Identification |
Result |
1. |
80% |
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2. |
90% |
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3. |
100% |
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4. |
110% |
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5. |
120% |
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Correlation
Coefficient (R2) |
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Sr. No. |
1 |
2 |
3 |
4 |
5 |
6 |
Result |
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Average |
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% RSD |
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Sr. No. | 1 | 2 | 3 | 4 | 5 | 6 |
Result |
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Average |
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% RSD |
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Details |
Repeatability |
Intermediate
Precision |
Analyst |
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Date |
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%
Assay of Azithromycin |
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Repeatability |
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Intermediate Precision |
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AVERAGE |
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SD |
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% RSD |
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CONCLUSIONS
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