SOP on Sampling of Raw Material
Objective: To lay down the procedure for sampling of raw material.
Scope: This procedure is applicable for sampling of raw material
Responsibility: Chemist or above
Accountability: Head – Quality Control
Procedure:
Sampling of Raw Materials:
Raw material sampling shall be initiated after receiving the “GRN” from warehouse.
Ensure that material is received from manufacturer mentioned in Approved Vendor List.
QC personnel shall enter the material details mentioned in received GRN from warehouse in raw material control register and allot A.R. No.
QC Section In Charge shall allocate the sampling activity to trained QC personnel as per SOP.
QC Section-In-Charge shall issue required “SAMPLED” labels to QC personnel who is going to sample the material.
QC personnel shall go to the warehouse along with “Sampling Report of Raw Material”, GRN, labels (as per requirement). “sample for microbial analysis”, cleaned and dried sampling tools, container to collect samples (use sterile containers and sterile spatula’s to collect sample for microbiology testing).
QC personnel shall enter the details like activity to be performed, on the Status board of sampling area.
Monitoring of differential pressure, temperature and Relative Humidity shall be done on daily basis even if there is not any sampling activity.
QC personnel shall record the Differential pressure of the sampling area and ensure the observed reading is within the limits.
QC personnel shall enter into the Personnel air lock area and follow the gowning procedure as per SOP.
Ensure that the temperature and Relative Humidity of the sampling booth is within the limits and record the observations.
Check the status of the booth and ensure that a ‘CLEANED’ label duly filled and signed is displayed.
Operating procedure for RLAF:
Switch “ON” the light by pressing button on the panel.
Wait till the differential pressure shows the constant pressure drop.
Ensure that the differential pressure gauges show the following pressure drop as below:
| Type of filters | Filters | Pressure Differential (mm of water) |
| Pre- filter | 10 µ Pre-filter | 1 – 5 mm |
| Fine-filter | 5 µ Fine- filter | 5 – 10 mm |
| HEPA-filter | 0.3 µ (HEPA) | 10 – 20 mm |
In case the differential pressure across pre-filter goes below 1 mm or exceeding 5 mm of water; sampling activity shall not be carried out. Inform the Engineering Depts. to rectify the fault & ensure the limits before starting of the sampling activity.
In case the differential pressure across fine filter goes beyond 10 mm of water, no sampling activity shall be carried out as fine filters may be clogged. Inform the Engineering Depts. to rectify the fault & ensure the limits before starting the sampling activity.
In case the differential pressure across HEPA filter goes beyond 20 mm of water, no sampling activity shall be carried out as the HEPA filter(s) may be clogged. Inform the Engineering Depts. to check the HEPA filter(s) & rectify the fault by changing the same (if applicable).
Lower pressure drops indicate malfunctioning of motor, blowers or grossly leaking or by passed filters.
Ensure that laminar airflow is switched ‘’ON’’ for a minimum of 15 minutes before the start of sampling operations.
Switch ON the balance and carry out sampling within safe working zone (blue color line).
On completion of activity Switch “OFF” the balances.
Switch “OFF” the light by pressing button on the panel.
Switch “OFF” the mains electric supply.
Precaution At the end of sampling:
Switch “OFF” the balances.
Switch “OFF” the light by pressing button on the panel.
Switch “OFF” the blower motors by pressing button on the panel.
Switch “OFF” the mains electric supply.
Manometer of Reverse Laminar Air Flow is to be checked before starting the air flow. The manometer level should be at “zero” position. The RLAF shall be kept on at least 15 minutes before start of sampling. Operate the RLAF as per SOP.
Record the sampling time and differential pressure of the RLAF in sampling operational log book..
QC personnel shall check cleanliness of the each container to be sampled and clean if necessary prior to sampling.
QC personnel shall check each material container label for details mentioned on against received GRN.
QC personnel shall have to ensure that “Quarantine” labels are affixed as per SOP, by warehouse department and check the details against GRN. Sampling of non-sterile solids shall be carried out under RLAF located in sampling area of warehouse.
Sampling of liquid materials shall be done in the area dedicated for liquid sampling.
Sampling of sterile materials shall be done as per SOP..
Sampling devices shall be wrapped in aluminum foil with status label “Cleaned and Ready for Use”. And shall be covered with poly bag .
Before sampling activity QC personnel shall cover the sampling tools with another poly bag (double cover) and shall carry to sampling area and remove the outer cover before entering into the sampling booth.
Material to be sampled shall be brought into sampling booth through material air lock.
QC personnel shall use sampling tools as follows:
| Type of Raw material | Tools | Sample collection container |
| Solid material | SS sampling rod / SS spatula | LDPE bag |
| Liquid material | SS scoop | Glass container with glass stopper |
Each sampling device has unique Identification No. shall be allotted to each sampling device.
Identification No. shall be assign as QCSSP-XX
Where;
QC stands for Quality control
SSP stands for Stainless steel Spatula / Rod / Scoop
XX stands for sequential number starts from 01.
QC personnel shall open the containers or bags under the RLAF individually and take out the sample approximately.
To change Pharmacopoeial grade of approved raw material or to test same raw material in more than one Pharmacopeial grade, then warehouse shall have to send different GRN for test required as per Pharmacopeia.
Additional sampling quantity shall be calculated and recorded as per annexure no.: QCSP011/A03 and analytical activity shall be referred from SOP.
Sampling Plan:
Before taking the container(s) inside, ensure that the container(s) are clean. If any container is found damaged or with broken / tampered seal then the container shall be
rejected and the same shall be informed to the In-charge of Warehouse department.
Observe visually the appearance of the material for any abnormalities like discoloration, lumps, non-characteristic odour, foreign matter, physical heterogeneity etc.
Material of only one batch number shall be sampled at a time. After sampling of each material cleaning shall be done as per SOP.
Withdraw the sample from the no. of containers as per the table given below:
| Type of Material | No. of Containers | Type of sample |
| Inactive | √n + 1 of the total container | Composite Quantity (for analysis & for retention sample) & From each sampled container (for identification) |
| Active | 100 % of total containers | Composite Quantity (for analysis & for retention sample) & From each container (for identification) |
If number of containers of inactive materials are five or less than five then each individual container shall be sampled.
100 % sampling shall be done in case of inactive material received from vendors, whose site has not been inspected for list of vendors, whose site has not been inspected.
Container number of each container shall be assigned as x/y where x is serial number of container and y is the total number of containers, e.g. 1/10 shall be assigned for first container out of 10 containers.
QC personnel shall open the containers or bags under the sampling booth and withdraw approximate quantities as per list prepared for active materials and for inactive materials.
List for sample quantity of active and inactive raw material shall be prepared and reviewed by QC department and approved by QA department. Quantity to be sampled shall be as per approved list. Document No. shall be assigned to the list for active material and for inactive materials, where XX is for version no. List shall be revised, if sample quantity of any material has to change or new material has to be added in the list.
Raw materials of specific nature are to be sampled with care, (where its potency, characters, stability are related with storage conditions, i.e. specific temperature, humidity, light resistant or any such requirements).
For composite sample, withdraw quantity of sample as per list of sample quantity, with sampling rod from individual containers ensuring that sample approximately equal quantity are drawn from individual containers.
Sample shall be collected from top, middle & bottom of the layers from the drums for solid materials and for liquid/solvent, top and bottom portion of the barrel / containers. In case of any abnormalities observed, inform to QA Officer for necessary action.
Mix the top, middle and bottom portion of solid raw material sampled in S.S. sampling pan. Separately weigh and make composite sample for analysis & retention sample. Transfer the material into two LDPE polybag and weigh. Affix label “SAMPLE FOR ANALYSIS” & “SAMPLE FOR RETENTION” on LDPE polybag. Label shall be ‘SAMPLE FOR ANALYSIS’ , ‘’RETENTION SAMPLE’’.
For identification sample, withdraw quantity of sample as per list of sample quantity, with spatula from individual containers and transfer the material into LDPE (Low density polyethylene) polybag and weigh. Affix label “SAMPLE FOR IDENTIFICATION” on each LDPE polybag. Label shall be mentioning containers number.
Properly close the container(s) under RLAF and affix self-adhesive label of “SAMPLED” mentioning container number.
Record all observations in sampling report of raw material.
Cleaning of Sampling Devices:
Sampling devices shall be washed with running purified water. During washing of the sampling devices, if any residue is visually seen, scrub the sampling devices with brush and wash it thoroughly with purified water.
After removal of all residues from the sampling devices, rinse the sampling devices thoroughly with purified water and shall wrap in double polybag. Washed sampling devices wrapped in polybag shall be brought to QC for drying.
Drying shall be done in hot air oven at 60°C for 1 hour/using air dryer. After completion of drying, wrap the sampling devices in aluminum foil and put “CLEANED & READY FOR USE” status label.
Cleaned sampling devices shall be stored in SS sampling tool box.
Record the cleaning activity in cleaning and usage log for sampling devices.
Bring the sampled polybags/Glass Bottles to Quality Control Laboratory for analysis.
List of Annexure / Formats:
- Raw material Control Register
- Sampling report of raw material
- Sampling operational log book
- Label of Sample for Analysis
- Label for Retention Sample
- Sampled quantity for raw material (active)
- Sampled quantity for raw material (inactive)
- Label for Sampled
- Label for Cleaned & Ready for Use
- Format of Cleaning and usage log book for sampling devices
- Label of Sample for Microbial Analysis
- Label of sample for Identification
- Record for differential pressure
- Temperature and Relative Humidity Record by digital hygrometer