SOP for Qualification of Reagents Used in Analytical Method Development
| Department | Analytical Method Development |
|---|---|
| SOP No. | SOP/AMD/036/2025 |
| Supersedes | SOP/AMD/036/2022 |
| Page No. | Page 1 of 14 |
| Issue Date | 19/05/2025 |
| Effective Date | 20/05/2025 |
| Review Date | 19/05/2026 |
1. Purpose
This SOP defines the procedure for qualifying reagents used in the Analytical Method Development (AMD) department. The aim is to ensure that all reagents used for method development and validation are appropriate for their intended use, traceable, and conform to applicable regulatory and GMP standards.
2. Scope
This SOP applies to all chemical reagents, buffers, indicators, titrants, and solvents used in the AMD laboratory for developing, optimizing, or validating analytical procedures for APIs, excipients, and formulations.
3. Responsibilities
- Analytical Scientist: Selects and initiates qualification for new or critical reagents used in method development.
- QA: Reviews and approves reagent qualification records and ensures traceability.
- Store Personnel: Ensures proper storage and labeling of reagents with status tags.
- Head – AMD: Approves qualified reagent status and resolves any discrepancies.
4. Accountability
The Head of AMD is accountable for ensuring that only qualified reagents are used in the development and validation of analytical methods.
5. Procedure
5.1 Reagent Selection
- All reagents shall be of analytical reagent (AR), HPLC, or GC grade, unless otherwise justified.
- Reference supplier specifications, compendial monographs, and material safety data sheets (MSDS).
- Assign a unique Reagent ID number and document in Annexure-1: Reagent Qualification Log.
5.2 Receiving and Preliminary Inspection
- Inspect reagents upon receipt for:
- Supplier name and batch number
- COA availability and compliance
- Expiry date, manufacturing date, and packaging integrity
- Initial assessment to be recorded in Annexure-2: Reagent Receipt and Inspection Checklist.
5.3 Reagent Testing and Verification
- If COA is available:
- Verify identification and assay using one or more analytical techniques (UV, IR, titration)
- Compare values against pharmacopeial or internal specifications
- If COA is not available or if reagent is critical (e.g., titrant, pH modifier):
- Conduct full qualification testing as per Annexure-3: Reagent Testing Record
- Qualified reagents shall be assigned a status tag: “Qualified for Use in AMD”
5.4 Labeling and Documentation
- Each reagent container shall have a legible label stating:
- Reagent name
- Reagent ID
- Date of opening
- Use before date
- Qualified By & Date
- Update the Reagent Master List and qualification tracker maintained by QA.
5.5 Retesting and Requalification
- Retest intervals:
- 6 months for aqueous buffers
- 12 months for acids, bases, or non-volatile solvents
- Requalification to be documented in Annexure-4: Reagent Requalification Form.
5.6 Storage and Handling
- Store qualified reagents in clean, ventilated chemical cabinets at designated temperature and humidity conditions.
- Highly sensitive reagents (e.g., perchloric acid, iodine) to be stored with additional secondary containment.
- Maintain usage logs for critical reagents in Annexure-5: Critical Reagent Usage Log.
5.7 Non-Conformance Management
- If reagent fails qualification:
- Label as “Rejected”
- Segregate and record deviation in accordance with SOP/QMS/042/2025
- Perform impact analysis for any methods developed using unqualified reagents.
6. Abbreviations
- AMD: Analytical Method Development
- QA: Quality Assurance
- COA: Certificate of Analysis
- MSDS: Material Safety Data Sheet
- SOP: Standard Operating Procedure
7. Documents
- Reagent Qualification Log – Annexure-1
- Reagent Receipt and Inspection Checklist – Annexure-2
- Reagent Testing Record – Annexure-3
- Reagent Requalification Form – Annexure-4
- Critical Reagent Usage Log – Annexure-5
8. References
- ICH Q7 – Good Manufacturing Practice for Active Pharmaceutical Ingredients
- USP General Chapter <841> – Specific Gravity
- WHO TRS 986 Annex 2 – Good Practices for Quality Control Laboratories
- 21 CFR Part 211.84 – Testing and Approval of Components
9. SOP Version
Version: 2.0
10. Approval Section
| Prepared By | Checked By | Approved By | |
|---|---|---|---|
| Signature | |||
| Date | |||
| Name | |||
| Designation | |||
| Department |
11. Annexures
Annexure-1: Reagent Qualification Log
| Reagent ID | Reagent Name | Supplier | Batch No. | Qualification Date |
|---|---|---|---|---|
| RG-2025-017 | Sodium Hydroxide | Rankem | NA25K7 | 02/05/2025 |
Annexure-2: Reagent Receipt and Inspection Checklist
| Parameter | Status | Remarks |
|---|---|---|
| COA Present | Yes | Verified |
| Packaging Intact | Yes | No leakage |
| Expiry Date | Valid | Dec 2026 |
Annexure-3: Reagent Testing Record
| Test Performed | Method | Result | Status |
|---|---|---|---|
| Identification (IR) | USP | Matches spectrum | Pass |
Annexure-4: Reagent Requalification Form
| Reagent ID | Requalification Date | Test Performed | Status |
|---|---|---|---|
| RG-2025-012 | 05/11/2025 | pH Adjustment Efficiency | Pass |
Annexure-5: Critical Reagent Usage Log
| Date | Reagent ID | Analyst | Purpose | Remarks |
|---|---|---|---|---|
| 06/05/2025 | RG-2025-017 | Ajay Verma | Titration Buffer Prep | Used as per SOP |
Revision History:
| Revision Date | Revision No. | Details | Reason | Approved By |
|---|---|---|---|---|
| 04/05/2025 | 2.0 | Added new annexures for requalification and usage tracking | GMP audit compliance |