SOP on Sampling of Raw Material
- To lay down the procedure for the sampling of raw material.
- This procedure is applicable for the sampling of raw material.
- Chemist or above
- Head – Quality Control
- Sampling of Raw Materials:
- Raw material sampling shall be initiated after receiving the “GRN” from the warehouse.
- QC personnel shall enter the material details in the raw material control register and allot A.R. No.
- QC personnel shall generate labels of “SAMPLED”.
- QC personnel shall generate labels of “UNDER TEST “. The no. of ‘UNDER TEST’ labels shall be ‘no. of container(s) + 1’.
- If the number of containers is five then six-under test labels shall be taken out and one label will be numbered as 00 of 05, 00 of 05 for specimen label with sampling report, and 01 of 05 for container number 01, 02 of 05 for container number 02 and so on.
- QC personnel shall go to the warehouse along with ‘Sampling Report of Raw Material’, GRN, Sampled labels, and Under Test labels.
- QC personnel shall check the material as per GRN.
- QC personnel shall have to ensure that “Quarantine” labels are affixed on each unit pack by the warehouse department.
- QC personnel shall enter into the sampling booth as per SOP and Check the status label “CLEANED AREA” on the sampling booth before entering into the sampling booth.
- Ensure that the Differential pressure of the sampling booth is within the limits and record the observations.
- Ensure that the temperature and Relative Humidity of the sampling booth is within the limits and record the observations.
- The manometer of Reverse Laminar Air Flow is to be checked before starting the airflow. The manometer level should be at a “zero” position. The RLAF shall be kept on at least before 15 min of start of sampling. Operate the RLAF as per SOP.
- Record the sampling start time and differential Pressure of the RLAF in the sampling operational logbook.
- A sampling of non-sterile solid shall be carried out under RLAF located in the sampling area of the warehouse. Sampling of liquid materials shall be done in the area dedicated for liquid sampling.
- QC person shall use cleaned and dried Sampling devices. These sampling devices shall be wrapped in aluminum foil with the status label “Cleaned and Ready for Use”.
- QC personnel shall use sampling utensils as follows
|Type of Raw material||Utensils||Sample collection container|
|For liquid sampling from drum / bag / container||S.S. sampling rod||Glass bottles|
|For liquid sampling from bottles.||S.S. sampling rod||Glass bottles|
|For sampling of material from solid bulk containers.||SS sampling rod / SS spatula||LDPE bag|
- QC personnel shall open the containers or bags under the sampling booth individually and take out the sample as per sampling plan.
- 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||1. Composite Quantity (for analysis & for retention sample)
2. From each sampled container (for identification)
|Active||100 % of total containers||1. Composite Quantity (for analysis & for retention sample)
2. From each container (for identification)
- If no. of containers of inactive materials are five or less than five then each individual container shall be sampled.
- 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 the first container out of 10 containers.
- Put the container number on label affixed on sample for identification.
- QC personnel shall open the containers or bags under the sampling booth and withdraw quantities 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.
- List shall be revised, if sample quantity of any material has to change or new material has to be added in the list.
- The sample shall be collected from the 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 in the S.S. sampling pan and transfer the required material for identification in LDPE (Low-density polyethylene) polybag.
- In raw materials where microbiological testing is required, the sample is to be drawn in a separate glass vial bearing the label “SAMPLE FOR MICROBIAL ANALYSIS” from every sampled container. Label of Sample for Microbial Analysis.
- The glass vial and spatula for the micro-sample should be sterile.
- 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 resistance, or any such requirements).
- For composite samples, withdraw the appropriate quantity of sample equivalent to the required quantity from individual containers ensuring that approximately equal quantities are drawn from individual containers.
- Fill the required quantity from the composite sample for “RETENTION SAMPLE” as well as for “SAMPLE FOR ANALYSIS”.Label the samples as ‘SAMPLE FOR ANALYSIS’ , ‘’RETENTION SAMPLE’’.
- Properly close the container(s) under RLAF and affix the self-adhesive label of “SAMPLED”.
- Affix self-adhesive label of “UNDER TEST” on all containers of that batch.
- Record all observations in the sampling report of raw material.
- Cleaning of Sampling Utensils:
- Sampling Utensils shall be washed with running purified water.
- During washing of the sampling Utensils, if any residue is visually seen, scrub the sampling Utensils with a lint-free cloth and wash it thoroughly with purified water.
- After removal of all residues from the sampling Utensils, rinse the sampling Utensils thoroughly with purified water and finally rinse the sampling Utensils with Isopropyl alcohol and dry it.
- After completion of drying, wrap the sampling Utensil in aluminum foil and put the “CLEANED & READY FOR USE” status label.
- Keep the sampling Utensils in a designated place.
- Record the cleaning activity in cleaning and usage log for sampling Utensils.
- 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 logbook
- 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 ‘UNDER TEST’
- Label for ‘Cleaned & Ready for Use’
- Format of Cleaning and usage logbook for sampling devices
- Label of Sample for Microbial Analysis
- Label for Identification
- References (if any):
- ICH Q7
- Reason for Revision:
- Not Applicable
- SOP: Standard Operating Procedure
- QC : Quality Control
- QA : Quality Assurance
- SG : Sub general
- R. No.: Analytical Report No.
- GRN : Goods Receipt Note
- LDPE : Low density polyethylene
- S sampling device : Stainless steel sampling device
- IPA : Isopropyl Alcohol
- cGMP : Current Good Manufacturing Practice
- cGLP: Current Good Laboratory Practice
END OF SOP