release characteristics over time for different formulations under discriminatory dissolution conditions.

2. Scope

This SOP applies to all oral solid dosage forms including immediate-release, sustained-release, delayed-release, and modified-release products that are developed in the Analytical Method Development (AMD) laboratory.

3. Responsibilities

• Analytical Scientist: Executes dissolution runs, collects samples, and calculates release profiles.
• Formulation Scientist: Provides formulation composition, target release rate, and supports discriminatory study design.
• Reviewer: Verifies data integrity and profile modeling accuracy.
• Head – AMD: Approves the finalized drug release profile and reports.

4. Accountability

The Head of Analytical Method Development is accountable for ensuring accurate, reproducible, and regulatory-compliant development of dissolution profiles for all test formulations.

5. Procedure

5.1 Prerequisites and Setup

1. Ensure finalized:
   • Dissolution medium (refer SOP/AMD/101)
   • Sink conditions confirmed (refer SOP/AMD/102)
   • Apparatus selected (refer SOP/AMD/103)
2. Calibrate dissolution instrument and verify temperature at 37 ± 0.5°C.
3. Prepare API working standard and validate analytical method for dissolution sample quantification.
4. Record all setup parameters in Annexure-1: Profile Run Setup Log.

5.2 Sample Loading and Initial Testing

1. Weigh and dose six dosage units (e.g., tablets or capsules) into each vessel.
2. Use 900 mL medium in each vessel unless otherwise justified.
3. Maintain agitation as per method (typically 50–100 rpm for paddles or baskets).
4. Record formulation details in Annexure-2: Dosage Form Input Log.

5.3 Sampling Strategy

1. Select appropriate time points to capture full release kinetics:
   • Immediate-release: 5, 10, 15, 30, 45, 60 minutes
   • Extended-release: 1, 2, 4, 6, 8, 12, 24 hours
2. Withdraw 10 mL sample at each time point, replacing with equal pre-warmed fresh medium.
3. Filter each sample using 0.45 µm filters.
4. Record sampling details in Annexure-3: Sampling Log Sheet.

5.4 Sample Analysis

1. Analyze each sample using validated UV or HPLC method.
2. Prepare a calibration curve and bracket samples with standard solutions.
3. Calculate % drug released = (Sample Conc. / Label Claim) × 100.
4. Document in Annexure-4: Analytical Results Table.

5.5 Data Compilation and Profile Plotting

1. Plot mean % drug released (Y-axis) versus time (X-axis) for n=6 units.
2. Calculate:
   • Mean and % RSD at each time point
   • f2 similarity factor if comparing profiles
   • T50%, T90%, AUC if required
3. Evaluate profile reproducibility and discriminatory capability.
4. Compile graphs and values in Annexure-5: Dissolution Profile Summary.

5.6 Acceptance Criteria

1. For IR products: ≥ 85% drug release in 30 minutes unless otherwise justified.
2. For SR/ER: Release profile should match design intent and demonstrate controlled release.
3. % RSD ≤ 10% for all time points.
4. Discriminatory nature of profile must be demonstrated across formulation variants.

5.7 Reporting and Archival

1. Compile all annexures, graphs, and observations in a report format.
2. Review by QA and final approval by Head – AMD.
3. Archive electronic and printed versions of data as per data integrity SOP.

6. Abbreviations

• IR: Immediate Release
• SR: Sustained Release
• ER: Extended Release
• RSD: Relative Standard Deviation
• AUC: Area Under Curve
• f2: Similarity Factor
• SOP: Standard Operating Procedure

7. Documents

1. Profile Run Setup Log – Annexure-1
2. Dosage Form Input Log – Annexure-2
3. Sampling Log Sheet – Annexure-3
4. Analytical Results Table – Annexure-4
5. Dissolution Profile Summary – Annexure-5

8. References

• USP <711> – Dissolution
• FDA Guidance for Industry: Dissolution Testing of Immediate Release Solid Oral Dosage Forms
• ICH Q2(R1) – Validation of Analytical Procedures

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: Profile Run Setup Log

Media	Apparatus	Volume	RPM	Bath Temp
pH 6.8 buffer	Paddle	900 mL	50	37°C

Annexure-2: Dosage Form Input Log

Formulation	Batch No.	Dose	Label Claim
Test Tablet A	TT-A/01	1 Tablet	100 mg

Annexure-3: Sampling Log Sheet

Time (min)	Sample Volume (mL)	Replaced Volume (mL)	Filtered?	Analyzed?
5	10	10	Yes	Yes

Annexure-4: Analytical Results Table

Time (min)	Mean % Released	% RSD
30	87.2%	3.2%
45	93.5%	2.7%

Annexure-5: Dissolution Profile Summary

The formulation showed a rapid and complete drug release with > 85% release at 30 min. RSD across all time points remained below 5%. Based on the data, the method is considered robust and suitable for QC release testing.

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
04/05/2025	2.0	Expanded procedure, updated annexures, added f2 comparison guidance	Annual Review