sop for sampling of intermediates and finished products

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4 years ago

sop for sampling of intermediates and finished products

1.0 OBJECTIVE:

The objective of this SOP is:
1.1 To describe the procedure for sampling of intermediates and finished products during manufacturing operations.

2.0 RESPONSIBILITIES:

2.1 Quality Assurance Officer / Executive shall be:
2.1.1 Responsible for withdrawal of samples of Intermediates and Finished products on receipt of intimation from production.
2.1.2 Responsible for sending the collected sample with Sample advice slip to Quality Control for analysis.

3.0 ACCOUNTABILITY:

Head – Quality Assurance

4.0 PROCEDURE:

4.1 Preparation:
4.1.1. On receipt of Request for Analysis from production check that the BMR is completed up to that stage and all

the manufacturing steps are followed and documented including stage wise yields.
4.1.2. Ensure availability of clean spoon, clean bottles, vials, polybags, labels etc.
4.1.3. Prepare a sample label, which should contain following information.
a. Product name
b. Batch No.
c. Mfg . Dt . Exp. Dt :
d. Stage
e. Test
f. Sampled by.
g. Date of sampling

4.1.4. Affix the label on container to be used for sampling i.e. polybag in case of powder, tablets and capsules and glass container in case of liquids.

4.1.5. Wear latex hand gloves and nose masks.
4.1.6. Ensure that all the bulk container carry ‘STAGE’ labels with correct product and batch details.

4.2 Sampling Of Intermediates (Sterile):

4.2.1 Sterile Blend sampling will be done by Quality Officer( Microbiologist ) as per SOP No: A/QA/041.

4.3 Intermediate (Non-Sterile):

4.3.1 Open the container and withdraw equal quantity of sample from all the containers to make a pool sample as quantity mentioned below.

NOTE:
Core Tablets / capsules for Dissolution test should be sent after ensuring compliance of
physical parameter against limits as mentioned in BMR.

Sr. No.	Dosage Form	Sample quantity (Approximately)
1.	Capsules (Blend / Granules)	15.0 gm
2.	Tablets (Blend / Granules)	15.0 gm
3.	Dry syrup Sugar for LOD	5.0 gm
4.	Dry syrup (Blend Granules)	30.0 gm
5.	Dispersible tablet (Blend / Granules)	15.0 gm
6.	Core Tablets for Dissolution	20.0 No.

4.3.2 In case of bulk requiring the test of bulk density & particle size 20 gm extra sample per test shall be sent.

4.4 Non Sterile Liquids
4.4.1 Open the container and withdraw the sample with help cleaned silicon tube in clean dry glass container.
4.4.2 For light sensitive products sample container should be wrapped with Aluminium foil or black paper.
4.4.3 In case of Water for Injection collect the sample directly from solution preparation tank with help of cleaned silicon tube in cleaned glass container.
a. Sample Qty Bulk samples – 50 ml Approximately
b. Water for injection for bulk Mfg – 500 ml Approximately.

4.5 FINISHED PRODUCT SAMPLING:

4.5.1 Dry Syrup / Liquid Orals
4.5.1.1 Based on the following sample plan draw equal number of samples of filled bottles to represent start, middle and end of the filling operation so that the total numbers of sampled bottles, at the end of the batch is at least equal to the sample size required by the quality control lab.
1. Liquid Oral
a. 30ml Bottles – 10 Nos.
b. 50ml Bottles – 10 Nos.
c. 60ml Bottles – 10 Nos.
d. 100ml Bottles – 10Nos.
e. 200ml Bottles – 10 Nos.
2. Dry Syrup – 20 Nos

• In case of dry syrup requiring the test of content uniformity 10 bottles extra-shall be sent.
• In case of dry syrup requiring the microbiological test, 2 bottles extra shall be sent.

4.5.2 VIALS
4.5.2.1 In case of sterile dry powder and liquid vials draw equal number of samples from the start of filling operation

and thereafter at hourly interval till the end of the filling operation or if there any intervention so as to have requisite number of total samples indicated below
a. Sterile dry powder vials : 50 Nos.
b. Liquid vials (2ml) : 25 Nos.

4.5.2.2 The first two filled at the start of filling operation shall be sampled and thereafter-adequate number of samples

should be withdrawn at hourly intervals. Also last two units filled at the end of filling operation shall be sampled
Note:
Incase of export product, Quality Officer ( microbiologist) shall collect sample sas per SOP No: A/QA/041at aseptic area for

all API container used in filling for identification and sterility testing.

4.5.2.3 Store the collected samples in labeled container/polybag.
4.5.2.4 And send the collected sample to quality control for analysis.
4.5.2.5 Incase of Injectable products requiring the test of particulate matter as per USP, additional number of following samples should be sent.
a. Liquid vials 1ml, 2ml – 40 vials
b. Liquid vials 5ml, 10ml – 20 vials

4.5.3 TABLETS/ CAPSULES

4.5.3.1 Collect samples from the containers to make pool sample, based on following sampling plan.

No. Of containers Containers to be sampled
0 to 5 vials All
6 to 15 5
16 & above ^n +1
Note:
Collect sample from containers in such a way that the sample is representative of whole batch.

4.5.3.2 If the coating is carried out in more than one lot, withdraw equal quantity of sample
from each lot and make pool sample.
4.5.3.2 In case of tablet / capsules requiring the microbiological test, 40 tablets/ capsules be sent.

4.5.4 AMPOULES:

4.5.4.1 The number of samples to be down shall be as follows
a. 1 ml : 125 No. per lot
b. 2 ml : 100 No. per lot
c. 3 ml : 80 No. per lot
d. 5 ml : 80 No. per lot
e. 10ml : 80 No. per lot
f. 15ml : 50 No. per lot

4.5.4.2 Incase of Injectable products requiring the test of particulate matter as per USP,
4.5.4.3 Additional number of following samples should be sent.
a. 1 ml ampoules : 50 Nos.
b. 2 ml & 3ml ampoules : 25 Nos.
c. 5 ml, 10 ml & 15 ampoules : 20 Nos.

4.5.4.4 For aseptically filled ampoules / vials.
4.5.4.5 The first two units filled at the start of filling operation shall be sampled.
4.5.4.6 Thereafter adequate number of samples should be withdrawn at hourly intervals and units filled at the end of filling operation shall be sampled
4.5.4.7 Store the collected samples in labeled containers/ polybag.
4.5.4.8 Send the filled containers to Quality Control Laboratory. Ensure that they are not less than required quantity.
4.5.4.9 For terminally sterilized ampoules
4.5.4.10 Draw equal number of samples from upper, middle and lower shelves of autoclave after sterilization cycle.

4.5.4.11 Ampoules shall be sampled from all four corners and center of upper, middle and lower shelves to form pool sample for microbiological as well as chemical analysis.
4.5.4.12 After sampling close the containers immediately.
4.5.4.13 Close the sample container/seal the polybag and record the details in BMR and sample request.
4.5.4.14 Send the sample and request for analysis to Quality Control Laboratory for testing.

5.0 REASON FOR REVISION:

This SOP is modified in order to be more effective in its responsibility and procedure.

6.0 TRAINING:
Trainer — Head – Quality Assurance
Trainee — Quality Assurance Officers

7.0 DISTRIBUTION:

Certified Copy No. 1 : Head of Department
Certified Copy No. 3 : Head of Department – Quality Control
Certified Copy No. 4 : Head – Plant Operations
Original Copy : Head – QUALITY ASSURANCE

8.0 ANNEXURES:

Nil.

9.0 REFERENCE:

In-house

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