# Analytical Procedure Validation Protocol

> Every bracketed field is a decision to make and record **before** data collection.
> `plan_validation.py --protocol` generates a framework-specific version of this document with the
> required characteristics already listed.

| Field | Value |
| --- | --- |
| Protocol number / version | [ ] |
| Analytical procedure identifier and version | [ ] |
| Product / analyte / matrix | [ ] |
| Measured quality attribute | [ ] assay / impurity (quantitative) / impurity (limit) / identity / other |
| Governing framework and section | [ ] |
| Regional expectation confirmed with | [ ] |
| Related development report (ICH Q14) | [ ] |
| Author / date | [ ] |
| Technical reviewer / date | [ ] |
| Quality unit approval / date | [ ] |

## 1. Intended purpose and analytical target profile

- Measurand and reporting unit: [ ]
- Decision the result supports: [ ] release / stability / in-process / clinical / other
- Specification or reporting limits served: [ ]
- Required reportable range, derived from the specification: [ ]
- Performance characteristics and criteria (the ATP): [ ]

## 2. Pre-stated acceptance criteria

State a numeric criterion and its justification for every characteristic to be validated. A
criterion with no justification traceable to the specification, the ATP, or development data is not
defensible.

| Characteristic | Criterion | Justification | Framework reference |
| --- | --- | --- | --- |
| Specificity / selectivity | [ ] | [ ] | [ ] |
| Response (calibration model) | [ ] | [ ] | [ ] |
| Lower range limit (DL / QL) | [ ] | [ ] | [ ] |
| Accuracy | [ ] | [ ] | [ ] |
| Repeatability | [ ] | [ ] | [ ] |
| Intermediate precision | [ ] | [ ] | [ ] |
| Combined accuracy and precision, if used | [ ] | [ ] | [ ] |

- Interval to be reported alongside accuracy and precision: [ ] confidence level [ ]
- Does the criterion apply to the point estimate or to the whole interval? [ ]

## 3. Study design

| Characteristic | Levels | Replicates | Runs / days / analysts / instruments |
| --- | --- | --- | --- |
| Response | [ ] (minimum 5 for ICH Q2(R2)) | [ ] | [ ] |
| Accuracy | [ ] | [ ] | [ ] |
| Repeatability | [ ] | [ ] | [ ] |
| Intermediate precision | [ ] | [ ] | [ ] |
| Lower range limit | [ ] | [ ] | [ ] |

- Replicate count matches the routine reportable result: [ ] yes / [ ] justified deviation: [ ]
- Calibration model and weighting, fixed in advance: [ ] unweighted / 1/x / 1/x² / non-linear / multivariate
- Randomisation and run order: [ ]
- Prior knowledge or development data used in place of a test, with justification: [ ]

## 4. Materials

| Item | Identity / grade | Lot | Assigned value and uncertainty | Expiry |
| --- | --- | --- | --- | --- |
| Reference material | [ ] | [ ] | [ ] | [ ] |
| Impurity standards | [ ] | [ ] | [ ] | [ ] |
| Blank / placebo matrix | [ ] | [ ] | — | [ ] |

## 5. Sample and solution handling

- Preparation procedure and dilution scheme: [ ]
- Solution stability window to be demonstrated: [ ]
- Storage conditions: [ ]

## 6. Specificity and stability-indicating properties

- Interferences to be challenged: [ ]
- Forced degradation conditions, if a stability-indicating claim is made: [ ]
- Orthogonal procedure, if used, and its accuracy: [ ]

## 7. Robustness (normally development, ICH Q14)

| Parameter | Nominal | Range varied | Effect assessed on |
| --- | --- | --- | --- |
| [ ] | [ ] | [ ] | [ ] |

## 8. Statistical treatment

- Software, version, and how calculations are verified: [ ]
- Handling of outliers, stated in advance: [ ]
- Scripts to be used and their output retained as records: [ ]

## 9. Deviations and data integrity

- Deviation identification, assessment and approval route: [ ]
- All results will be reported, including out-of-criteria values: [ ] confirmed
- Raw data location, audit trail, and review: [ ]

## 10. Approvals

| Role | Name | Signature | Date |
| --- | --- | --- | --- |
| Author | | | |
| Technical reviewer | | | |
| Quality unit | | | |