In-Process Sampling and Re-Sampling in Pharma

During manufacturing process Quality Assurance department Sampling on different stages and if result does not math they again sapling. In this blog post we study how In-Process Sampling and Re-Sampling in Pharma done by Q.A Department.

1. Purpose:

1.1. To establish a procedure for the In-process sampling during the manufacturing of all products.

2. Scope:

2.1. It is applicable to all the products being manufactured ____________ Pharmaceuticals.

3. Responsibilities:

3.1. QC Officer
3.2. Production Pharmacist
3.3. Q.A Officer
3.4. Lab Attendant

4. Procedure:

Sampling procedure and sample size is mentioned below for each process/stage:

4.1. GENERAL:

4.1.1. Quality Assurance Manager receives the request for analysis (F-04-05) from Production Department.
4.1.2. QA Officer/Lab Attendant checks/verify that the information given on requisition is correct or not according to process/stage.
4.1.3. QA officer/Lab Attendant wears mask and gloves before sampling, collects the sample in the presence of production pharmacist, as per status of the product.(Enter the sterile area as per specified protocol)
4.1.4. After Sampling QA officer/Lab Attendant label the sample with following information
4.1.4.1. Product name
4.1.4.2. Batch No.
4.1.4.3. Mfg. Date
4.1.4.4. Exp. Date
4.1.4.5. Stage
4.1.4.6. Date and Initial
4.1.5. Then send the sample along with sampling intimation slip to Q.C department for analysis.
4.1.6. QC analyst tests the sample and hands over the results to QC Manager.
4.1.7. QC Manager decides according to the results about the release or Rejection of the sample and intimates the QA and Production about the results.

4.2. INJECTABLES:

4.2.1. Water Sampling before ampoule/vial washing:
4.2.1.1. Before starting of the ampoule/vial washing sample of water is collected from the tank.
4.2.1.2. Take a washed dried glass vial. Rinse the vial 3 times with the same water to be sampled.
4.2.1.3. Take a sample of NLT 100ml for analysis.
4.2.1.4. Cover the vial with Al-foil to prevent environmental disturbances.
4.2.2. Distilled Water Sample Before Bulk Mixing:
4.2.2.1. Take 2 washed, dried glass vials.
4.2.2.2. Take a sample for distilled water of NLT 100ml in each vial from the storage tank and from the loop, after rinsing the glass vials with Distilled water 3 times.
4.2.2.3. Cover the vial with Al-foil to prevent environmental disturbances.
4.2.3. Bulk Mixing Stage:
4.2.3.1. After batch manufacturing take the sample from the mixing tank.
4.2.3.2. Verify the up-to-mark volume.
4.2.3.3. Take washed and dried glass vial.
4.2.3.4. Take a sample of NLT 100ml in vial.
4.2.3.5. Cover the vial with Al-foil to prevent environmental disturbances.
4.2.4. Start of Filling:
4.2.4.1. Issue line clearance as per SOP-08-001.
4.2.4.2. Take a sample of ampoule/vial from each nozzle of the filling machine.
4.2.4.3. Sample size should be NLT10 ampoules and NLT 5 vials.
4.2.5. Sampling for Sterility/Assay/LPC(liquid particle count):
4.2.5.1. Take a collective sample of NLT 50 ampoules and NLT 25 vials from the bulk after autoclave. (Optically Checked ampoules/vials for LPC)

4.3. ORAL SOLID DOSAGE FORMS (OSDs): (TABLET/CAPSULE)

4.3.1. Rinse Water Sample for Mixing tank:
4.3.1.1. After washing of mixing tank rinse it with water thrice.
4.3.1.2. Collect rinse sample of NLT 100ml in a washed and dried glass vial.
4.3.1.3. Cover the vial with Al-foil to prevent environmental disturbances.
4.3.2. Bulk Mixing Stage:
4.3.2.1. Take a plastic poly bag and sampling rod.
4.3.2.2. Collect a collective sample of 10gm from top, center and bottom of the container with the help of sampling rod.
4.3.3. Start of Tablet Compression/Capsule Filling:
4.3.3.1. Issue line clearance as per SOP-08-001.
4.3.3.2. Run the compression/filling machine for collection of sample.
4.3.3.3. Take a sample of NLT 50 tablets/capsule.
4.3.4. After Tablet Coating:
4.3.4.1. Take random sample of NLT 30 tablets from the bulk in a plastic polybag.
4.3.4.2. Sample of uncoated tablets to be taken after compression from the bulk
4.3.5. Sampling for Leakage Test (Blister Seal Test):
4.3.5.1. Issue line clearance as per SOP-08-001.
4.3.5.2. Take the sample of all blisters in one stroke.
4.3.5.3. Perform leakage test as per SOP-08-022.

4.4. LIQUID SYRUPS/SUSPENSIONS:

4.4.1. Rinse Water Sample for Mixing tank:
4.4.1.1. After washing of mixing tank rinse it with water thrice.
4.4.1.2. Collect rinse water sample of NLT 100ml in a washed and dried glass vial.
4.4.1.3. Cover the vial with Al-foil to prevent environmental disturbances.
4.4.2. Bulk Mixing Stage:
4.4.2.1. After batch manufacturing take the sample from the mixing tank.
4.4.2.2. Verify the up-to-mark volume.
4.4.2.3. Take washed and dried glass vial
4.4.2.4. Take a sample of NLT 100ml in vial.
4.4.2.5. Cover the vial with Al-foil to prevent environmental disturbances.
4.4.3. Start of Filling:
4.4.3.1. Issue line clearance as per SOP-08-001.
4.4.3.2. Take a sample from each nozzle of the filling machine.
4.4.3.3. Sample size should be NLT 8 bottles.

5. Re-Sampling:

5.1. In case of non-compliance of in-process test, QC Department issues the test report.
5.2. Q.A department will hold the in-process material by affixing HOLD label (LB-08-02).
5.3. Q.A Officer will re-sample the material, as per instruction of QC Department.
5.4. QC analyst will re-test/re-analyze the sample and intimates the QA regarding results.
5.5. Q.A Manager will decide about Release/rejection of the product.

6. In-Process Sampling and Re-Sampling in Pharma Controll Measure

• Ensure proper usage of PPEs while handling the materials
• Verify the upto mark volume from SMP before taking the sample
• Assign the numbers to nozzles and take the sample as 1,2,3…,etc
• Proper labeling with all necessary information of the product