Sampling and Testing in Exhibit and Process Validation Batches

1. Introduction

• Exhibit Batches: Produced at commercial scale (or pilot scale in some cases) before product launch, used to demonstrate manufacturing feasibility and generate stability, quality, and regulatory submission data.

• Process Validation (PV) Batches: Commercial-scale batches manufactured under normal operating conditions to confirm that the process consistently produces quality products meeting specifications.

• Sampling and testing are critical to verify process reproducibility, product quality, and GMP compliance.

2. Purpose of Sampling & Testing

• Demonstrate that the process is in a state of control.

• Provide scientific evidence for regulatory submissions (NDA, ANDA, dossiers).

• Support validation reports and continued process verification.

• Detect variability in raw materials, intermediates, and final products.

3. Sampling Plan Requirements

• Documented in Protocol: Sampling procedures, points, quantities, frequency, and rationale must be predefined in the Exhibit Batch or PV Protocol.

• Representative Sampling:

  • Raw materials and in-process materials

  • Blend uniformity samples

  • Critical process stages (granulation, drying, compression, coating, filling)

  • Packaging components (if applicable)

• Locations: Top, middle, bottom, and different areas of bulk material to ensure representativeness.

• Sample Size: Sufficient for initial testing, retain samples, and repeat testing if required.

4. Testing Parameters

For In-Process Samples

• Physical parameters: Moisture content, particle size, bulk density.

• Process parameters: Granulation endpoint, drying time/temp, blend uniformity.

• Weight variation, hardness, friability (for solid dosage).

• Assay and content uniformity.

For Finished Product

• Assay (potency)

• Dissolution

• Uniformity of dosage units

• Related substances / impurities

• Stability studies (accelerated & long-term)

• Microbial limits (if applicable)

5. Frequency of Testing

• Exhibit batches: Usually more frequent sampling at each critical stage.

• PV batches: Sampling as per validation protocol (often 3 consecutive commercial-scale batches).

6. Documentation Requirements

• Protocol approval by QA before execution.

• Batch Manufacturing Record (BMR) entries for each sampling/testing activity.

• Test results with acceptance criteria and reference to compendial or in-house methods.

• Deviations documented if any result falls outside protocol-defined limits.

• Final validation report summarizing all data.

7. GMP Compliance Points

• Sampling should be done using clean, labeled, GMP-compliant containers and tools.

• Maintain chain of custody for all samples.

• Follow ALCOA+ principles for data integrity.

• Samples and test results should be traceable to the specific batch, date, and person who performed the activity.

✅ Summary Flow:
Protocol Preparation → QA Approval → Sampling Execution → Testing & Recording → Data Review → Validation Report → Regulatory Submission.

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