SOP for Sampling of Raw Materials

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SOP for Sampling of Raw Materials

1.0 OBJECTIVE

To lay down a documented procedure for sampling of raw materials to ensure representative sampling, prevention of contamination, and compliance with Good Manufacturing Practices (GMP).

2.0 SCOPE

This procedure is applicable to the sampling of all raw materials (Active and Excipients) received at the warehouse and sampled by the Quality Control Department.

3.0 RESPONSIBILITY

3.1 Officer / QC Chemist and Above

  • Preparation of SOP
  • Sampling of raw materials
  • Documentation of sampling activities

3.2 Executive and Above

  • Review and checking of SOP

3.3 Head – QA

  • Approval of this SOP

4.0 ACCOUNTABILITY

Quality Control Head

  • Overall implementation and compliance with this SOP

5.0 DEFINITIONS

Raw Material Sampling:
The process of withdrawing a representative portion of material or a group of units from a larger quantity to determine its quality characteristics.

6.0 PRECAUTIONS, SAFETY & EHS

6.1 Precautions

  • Use cleaned and dried sampling equipment for each material.
  • Use clean, dry bottles with screw caps for liquid samples.
  • Use fresh polybags or clean dry bottles for solid samples.
  • For light-sensitive materials, use amber bottles or black polybags.
  • Ensure UV light is OFF during sampling (except during pre-sanitization exposure).
  • Sample only one batch at a time to prevent mix-up.
  • Ensure environmental conditions are within specified limits before sampling.

7.0 MATERIALS AND EQUIPMENT

7.1 Materials

  • 70% IPA solution
  • Sampling bags
  • “Under Test” and “Sampled” labels
  • Clean labeled sample containers (glass/plastic as applicable)
  • PPE (gloves, goggles, mask, gown)
  • 2.5% v/v disinfectant solution

7.2 Equipment

  • Spatula
  • Stainless Steel (SS) Sampling Rod
  • SS Liquid Sampler
  • Glass Pipette with rubber teat
  • RLAF (Reverse Laminar Air Flow) sampling booth

8.0 PROCEDURE

8.1 Cleaning of Raw Material Sampling Area

8.1.1 Floor Cleaning

  • Clean floor at the beginning and end of each shift using 2.5% v/v disinfectant solution.

8.1.2 Wall Cleaning

  • Clean walls weekly using a wet mop with 2.5% v/v disinfectant, followed by dry wiping.

8.1.3 RLAF Booth Cleaning

When sampling the same active (different batch numbers):

  • Perform dry mopping only.

When sampling different actives:

  • Perform wet mopping with 2.5% v/v disinfectant.
  • Follow with dry mopping.

After cleaning, QC personnel shall inspect the area and record observations in the sampling booth log.

8.2 Receipt of GRN

  • QC Chemist/Officer shall receive the GRN along with the Certificate of Analysis (COA) from the warehouse.
  • If COA is unavailable, inform Head QC. Sampling may proceed only after approval.
  • Vendor COA shall be reviewed against in-house specifications.
  • Record GRN details in Raw Material Inward Register:
    • GRN Number
    • Date
    • Material Name
    • Batch Number
    • Manufacturing & Expiry Date
    • Manufacturer & Supplier
    • Quantity Received

8.3 Physical Verification Before Sampling

  • Verify material details against GRN and vendor label.
  • Check number of containers and physical condition.
  • Record observations in Inspection Report.

Damaged Containers

  • Inform Head QC if container is damaged or seal is broken.
  • If inner packing is intact → Sampling may proceed from that container.
  • If inner packing is damaged → Container shall be rejected.

8.4 Sampling Plan

8.4.1 Active Raw Materials

  • Sampling from 100% of containers.

8.4.2 Excipients

  • If ≤ 4 containers → Sample 100%.
  • If > 4 containers → Follow 1 + √n method.

Example:
For 20 containers → √20 ≈ 4 → Sample = 1 + 4 = 5 containers.

8.5 Preparation for Sampling

Before starting sampling:

  • Ensure sampling booth and RLAF unit are cleaned and cleared.
  • Switch ON RLAF and UV light for 25–30 minutes.
  • Monitor environmental conditions:
    • Temperature: NMT 25°C
    • Relative Humidity: NMT 55%
    • RLAF Differential Pressure: 7–15 mm H₂O

If conditions are outside limits:

  • Inform Head Engineering & Head QC.
  • Sampling shall proceed only after rectification.
  • Ensure tools are cleaned and wrapped.
  • Clean outer surface of raw material container before entering booth.

8.6 Procedure for Sampling – Solid Raw Materials

  1. Bring container inside sampling booth.
  2. Open outer seal/stitches and inner packing carefully.
  3. Inspect for physical abnormalities:
    • Discoloration
    • Lumps
    • Foreign particles
    • Unusual odor
    • Heterogeneity

If observed → Inform Head QC immediately.

  1. For sterile materials:
    • Sampling shall be done from intact vials.
    • Do not open sterile bulk containers.

Using SS Sampling Rod

  • Ensure all cavities are closed.
  • Insert vertically to bottom (Position 1).
  • Rotate handle to open cavities.
  • Close cavities by reverse rotation.
  • Withdraw rod carefully.
  • Place horizontally; open cavities upward.
  • Collect sample using spatula into polybag.
  • Repeat for required sampling positions.
  • Pool sample where applicable.

Closing the Container

  • Expel air from inner polybag.
  • Secure tightly with tie band.
  • Close outer container properly.
  • Affix “SAMPLED” label.
  • Transfer container to designated area.

Identification Sampling

  • Active Materials: Identification from each container + pooled sample.
  • Excipients: Identification from each sampled container as per 1+√n plan.

8.7 Sampling Tools – Usage

Tool Application
SS Liquid Sampler Liquids from drums
Glass Pipette Liquids from bottles
Spatula Small solid containers (<5 kg)
SS Sampling Rod Solid materials in bags/drums

Spatula may be used for solid materials less than 5 kg.

8.8 Sampling Procedure – Liquid Raw Materials

  1. Wear appropriate PPE.
  2. Verify cleanliness of sampler and container.
  3. Label sample container as per SOP.
  4. Rinse sampler with sample liquid (if applicable); discard rinse.
  5. Open container under controlled conditions.
  6. Insert sampler at:
    • Top
    • Middle
    • Bottom
  7. Open sampler to collect liquid.
  8. Close sampler properly before removal.
  9. Transfer sample into labeled container.
  10. Minimize exposure to air (especially volatile materials).
  11. Seal container tightly (use parafilm/tamper seal if required).
  12. Clean liquid sampler after use.
  13. Store sample as per material requirement.
  14. Record details in Sampling Logbook.

8.9 Expiry Date Determination

If raw material is received with:

  • Manufacturing Date and Retest Date (but no expiry date),

Then expiry date shall be considered as five years from the date of manufacturing, unless otherwise specified by regulatory or stability data.

9.0 DOCUMENTATION

The following records shall be maintained:

  • Raw Material Inspection Report
  • Raw Material Inward Register
  • Raw Material Sampling Logbook
  • Sampling Booth Equipment Log

All entries shall be legible, signed, and dated.

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