Calibration of Dissolution Testing Apparatus in Pharmaceuticals

1. Introduction

The dissolution test is a critical quality control method in the pharmaceutical industry, ensuring drug release profiles meet pharmacopoeial requirements. Regular calibration of dissolution testing apparatus (e.g., USP Apparatus 1 – Basket and USP Apparatus 2 – Paddle) is essential for generating accurate and reproducible results.

2. Objective

• To verify that the dissolution apparatus operates within USP and ICH specifications.

• To ensure mechanical and performance suitability for routine analysis.

3. Principle

Calibration involves:

• Mechanical Calibration: Checking physical parameters like spindle speed, shaft wobble, vessel centering, paddle/basket alignment, and water bath temperature.

• Performance Verification Test (PVT): Using USP Prednisone Tablets (Reference Standard) to verify dissolution performance meets USP limits.

4. Mechanical Calibration Parameters (USP <711> & <724>)

1. Spindle Speed – Verify using a calibrated tachometer; must be within ±4% of the set value.

2. Vessel Centering – Center shaft within 2 mm of vessel axis.

3. Verticality (Shaft Wobble) – Maximum allowed run-out: 0.5 mm.

4. Paddle/Basket Height – Distance from bottom of vessel: 25 ± 2 mm.

5. Temperature – 37.0 ± 0.5°C in the dissolution medium.

6. Basket Integrity – Mesh intact, no deformation.

7. Vibration Check – No significant vibrations during operation.

5. Performance Verification Test (PVT)

• Conducted using USP Prednisone Reference Tablets.

• Follow USP method for medium preparation, degassing, and sampling.

• Compare dissolution results with USP acceptance range (e.g., mean % dissolved after specified time).

• PVT frequency: As per USP – typically every 6 months or after any major repair.

6. Documentation

• Equipment ID and serial number.

• Calibration date and due date.

• Details of mechanical checks and results.

• PVT raw data, calculations, and acceptance decision.

• Analyst and reviewer signatures.

7. Regulatory References

• USP <711> Dissolution

• USP <724> Drug Release

• FDA Dissolution Testing Guidance

• ICH Q2 (R1) – Analytical Validation