sop for sampling of sterile raw material

1.0 OBJECTIVE
To lay down a procedure for aseptic sampling of sterile Raw Material so as to get a
Representative sample of the whole lot for analysis.

2.0 RESPONSIBILITY

Quality Control Officer.

3.0 ACCOUNTABILITY

Quality Control Manager.

4.0 PROCEDURE

4.1 Generate Sampler’s checklist-RM as per the Batch Number mentioned in the Under Test list and decide the number of containers to be sampled as per sampling plan (Annexure – I).

4.2 Check and reconcile number of containers and the total quantity as shown in Under Test
Label. Compare the details like manufacturing date, expiry date and pharmacopoeia status mentioned on Sampler’s checklist-RM with that mentioned on manufacturer’s label. Ensure that each container is affixed with ‘UNDER TEST’ label. In case of any discrepancies inform to Quality Control Manager / Ware-House Manager.

4.1 Check the packing condition of the containers for any damages. Physically damaged
Containers shall not be considered for sampling and the same shall be Rejected..

4.2 In case of material received in triple laminated bags, the sample container received alongwith
the material shall be used for microbiological and chemical testing.

4.3 In case of sterile material received in aluminium containers, follow the procedure given
below,

4.5.1 Select the containers to be sampled and inform Ware-House Officer to transfer these containers to the raw material storage area of production block.

4.5.2 Sterilize and depyrogenate all sampling accessories as mentioned

4.5.3 Prepare label for individual container sample, with details of name of the material, Batch no., and container number.
4.5.4 Total number of labels to be prepared shall be equal to the number of containers to be sampled.

4.5.5 Prepare labels (annexure-II ) for Sample for Analysis, microbiology test and control sample.

4.5.6 Transfer the containers to the buffer zone. Follow the SOP on ‘Raw material receipt, storage, and transfer to sterile area’.

4.5.7 Enter into the sterile area following gowning and degowning procedure for sterile area.

4.5.8 Transfer the container to be sampled to the Quality Control Microbiology Lab ( Sterile Area.)

4.5.9 Ensure that temperature inside the room is less than 25 deg.C. & RH is less than 40% or as specified on Manufacturer’s label.

4.5.10 Place one container under LAF. Peel off the outer tape/seal from the mouth of the container and open the lid of the container aseptically.

4.5.11 Withdraw an appropriate quantity of sample aseptically into a piece of depyrogenated aluminium foil.

4.5.12 Observe carefully the physical appearance of the material for any abnormalities like discolouration, lumps, foreign matter and physical heterogeneity.

4.5.13 If any abnormalities are observed, collect the sample in two separate vial, for separate evaluation.

4.5.14 If no abnormalities are observed, transfer the sample equally into vials and simultaneously transfer approximately 1 gm sample in

the other vial for identification test from individual container before a pooled sample is taken for analysis.

4.5.15 Plug all vials with sterilized rubber plugs.

4.5.16 Close the lid of the container tightly, wrap the mouth with adhesive tape and remove the container from LAF booth.

4.5.17 Mark the sample containers using glass marker with batch number and container number in case of individual sample and only batch number in case of pool, control sample & micro sample.

4.5.18 Mark containers / packs which are selected for sampling with marker as N/1/n, N/2/n….N/S/n

(‘N’ stands for total number of packs / containers, ‘S’ for serial number of container selected for sampling and ‘n’ for total number of containers taken for sampling).

4.5.19 Similarly sample the rest of the containers aseptically. Refer annexure-II for total quantity to be sampled.

4.5.20 Seal all the vials with aluminium tear off seals.

4.5.21 Transfer all the containers to Air lock-1.

4.5.22 Transfer all the samples & sampling aids in the Air lock-1.

4.5.23 Clean the LAF bench and room and leave the sterile area alongwith the samples.

4.5.24 Label all the collected sample vials.

4.5.25 Affix ‘SAMPLED’ labels (Annexure – III) duly signed with date of sampling on the container.

4.5.26 Record all observations in the Sampler’s checklist-RM

4.5.27 Give the samples along with the Sampler’s checklist-RM, Supplier’s COA (if available) to Quality Control Laboratory for Chemical Analysis.

4.5.28 Inform the Ware-House Officer to shift all the containers back to Stores ‘UNDER TEST STORAGE’ area after performing decontamination of external surfaces.

5.0 Preparation of sampling accessories

5.1 Vials : Follow washing, drying, sterilizing and depyrogenate procedure as followed in normal production.

5.2 Rubber Stopper: Follow washing steam sterilization and drying procedure as followed in normal production run.

5.3 Spoons : Wash the spoon dry and wrap in 3 layers of aluminium foil, depyrogenate in Dry Heat Sterilizer at 250 degree Celsius for one hour.

5.4 Aluminium Foil : Cut pieces of aluminium foil of approximately 10cm.sq.area, wrap them in triple

layer of aluminium foil and depyrogenate in Dry Heat Sterilizer at 250 degree Celsius for one hour.

5.5 After depyrogenation of sampling accessories, transfer them to production block hatch.
Remove outer layer of wrap here, from this hatch transfer the accessories to aseptic area
hatch. Remove the second layer of the wrap and transfer them to buffer zone LAF.

6.0 ABBREVIATIONS :
SOP = Standard Operating Procedure
COA = Certificate of Analysis.

5.0 REFERENCES
In house

6.0 ANNEXURES :
Attached

ANNEXURE – I
SAMPLING PLAN

MINIMUM NUMBER OF CONTAINERS RECOMMENDED TO BE TESTED

Number of items in the batch	Minimum no. of containers to be sampled
Not more than100 containers	10% or 4 containers, whichever is greater
More than 100 but not more than 500 containers	10 containers
More than 500 containers	2% or 20 containers, whichever is least