SOP for Designing System Suitability Testing Parameters in Analytical Method Development

Department	Analytical Method Development
SOP No.	SOP/AMD/025/2025
Supersedes	SOP/AMD/025/2022
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 designing, validating, and documenting system suitability testing (SST) parameters during the analytical method development phase. System suitability ensures that the analytical system is functioning properly and can produce accurate and precise results prior to sample analysis.

2. Scope

This SOP applies to all chromatographic and spectroscopic analytical methods developed within the Analytical Method Development (AMD) department, including HPLC, GC, UV, and other analytical techniques requiring SST verification before analysis.

3. Responsibilities

• Analytical Scientist: Proposes SST parameters based on method performance and development data.
• Team Lead: Reviews justification for SST limits and ensures reproducibility.
• QA: Confirms SST acceptance criteria are documented and aligned with regulatory guidelines.
• Head – AMD: Approves final SST parameters for validation and routine application.

4. Accountability

The Head of AMD is accountable for ensuring all SST parameters are defined scientifically, verified through development data, and compliant with ICH, USP, and internal quality systems.

5. Procedure

5.1 Selection of SST Parameters

1. Define appropriate SST parameters based on the analytical technique and method requirements. Typical parameters include:
   • Chromatography: Resolution (Rs), Tailing Factor (T), Theoretical Plates (N), Retention Time (RT), %RSD of Peak Area
   • Spectroscopy: Absorbance drift, wavelength accuracy, baseline noise
   • General: Signal-to-noise ratio, peak symmetry
2. Record parameter selection in Annexure-1: SST Parameter Design Sheet.

5.2 Data Collection for SST Limit Definition

1. Conduct multiple system injections (minimum 6) during development trials.
2. Use qualified reference or working standard solutions.
3. Calculate statistical data: Mean, %RSD, min-max range.
4. Document raw data in Annexure-2: SST Trial Summary Log.

5.3 Establishing Acceptance Criteria

1. Apply the following general limits unless product-specific requirements dictate otherwise:
   • Resolution (Rs): ≥ 2.0
   • %RSD (Area): ≤ 2.0%
   • Tailing Factor: ≤ 2.0
   • Retention Time: Within ±2% of average
2. Include rationale for each limit based on method criticality, QbD outcomes, or historical control data.
3. List final acceptance values in Annexure-3: SST Acceptance Criteria Record.

5.4 Verification and Implementation

1. Verify SST performance across multiple analysts, instruments, and days.
2. Ensure repeatability and robustness of system parameters.
3. Include SST criteria in method validation protocol and report.
4. Update SOP/AMD/014/2025 (Method Development Report) to include SST design section.

5.5 Deviations and Trending

1. In case of SST failure:
   • Stop analysis
   • Perform investigation and document deviation
   • Retest with fresh standard or column
2. QA to evaluate if validation or method modification is required.
3. Trend SST values monthly using control charts to detect variability.

6. Abbreviations

• SST: System Suitability Testing
• Rs: Resolution
• RSD: Relative Standard Deviation
• RT: Retention Time
• QbD: Quality by Design
• USP: United States Pharmacopeia

7. Documents

1. SST Parameter Design Sheet – Annexure-1
2. SST Trial Summary Log – Annexure-2
3. SST Acceptance Criteria Record – Annexure-3

8. References

• ICH Q2(R2) – Validation of Analytical Procedures
• USP General Chapter <621> – Chromatography
• ICH Q14 – Analytical Procedure Development

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: SST Parameter Design Sheet

Method	Parameter	Reason for Inclusion
HPLC/AMD/071	Resolution	To differentiate API and impurity A
HPLC/AMD/071	%RSD	To ensure injection repeatability

Annexure-2: SST Trial Summary Log

Run	RT	Area	Rs	Tailing
1	5.83	102304	2.5	1.1
2	5.81	101998	2.4	1.2

Annexure-3: SST Acceptance Criteria Record

Parameter	Limit	Unit	Justification
Resolution	≥ 2.0	—	Ensures separation of peaks
%RSD	≤ 2.0	%	Acceptable repeatability threshold
Tailing Factor	≤ 2.0	—	Ensures peak symmetry

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
04/05/2025	2.0	Added annexures and included trending guidance	ICH Q14 compliance