Drugsformulations
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.
- QC personnel shall enter the material details in raw material control register as per Annexure No. 01 and allot A.R. No.
- QC personnel shall generate labels of “SAMPLED” as per Annexure No.08
- QC personnel shall generate labels of “UNDER TEST “as per Annexure No. 09 . The no. of ‘UNDER TEST’ labels shall be ‘no. of container(s) + 1’.
- If 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 as per Annexure No. 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’ as per Annexure No. 02 , 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 warehouse department.
- QC personnel shall enter into the sampling booth as per SOP. and Check the status label “CLEANED AREA” on sampling booth before entering into the sampling booth.
- Ensure that Differential pressure of the sampling booth is within the limits and record the observations as per Annexure No.03 .
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- Ensure that temperature and Relative Humidity of the sampling booth is within the limits and record the observations as per Annexure No. 01
- 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 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 sampling operational log book as per Annexure No. 03
- Sampling of non-sterile solid 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 .
- QC person shall use cleaned and dried Sampling devices. These sampling devices shall be wrapped in aluminum foil with status label “Cleaned and Ready for Use” as per Annexure No. 10
- 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 given .
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 first container out of 10 containers.
- Put the container number on label affixed on sample for identification. Label of ‘SAMPLE FOR IDENTIFICATION’ shall be as per Annexure No.13.
- QC personnel shall open the containers or bags under the sampling booth and withdraw quantities as per list prepared as per Annexure No.6 for active materials and Annexure No. 07 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 as QCSG01/D06-XX for active material and QCSG01/D07-XX 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.
- 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 in 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, 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 shall be as per Annexure No.12 .
- Glass vial and spatula for 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 resistant or any such requirements).
- For composite sample, withdraw appropriate quantity of sample equivalent to the required quantity from individual containers ensuring that approximately equal quantity are drawn from individual containers.
- Fill the required quantity from composite sample for “RETENTION SAMPLE” as well as for “SAMPLE FOR ANALYSIS”.
- Label the samples as ‘SAMPLE FOR ANALYSIS’ as per Annexure No.04’RETENTION SAMPLE’’ as per Annexure No.5
- Properly close the container(s) under RLAF and affix self-adhesive label of “SAMPLED” as per Annexure No.8 .
- Affix self-adhesive label of “UNDER TEST” as per Annexure No.9 on all containers of that batch.
- Record all observations in sampling report of raw material as per Annexure No.02
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 lint free cloth 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 finally rinse the sampling devices with Isopropyl alcohol and dry it.
- After completion of drying, wrap the sampling devices in aluminum foil and put “CLEANED & READY FOR USE” status label as per Annexure No. 10
- Keep the sampling devices in a designated place.
- 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 : Annexure 1
- Sampling report of raw material : Annexure 2
- Sampling operational log book :Annexure 3
- Label of Sample for Analysis : Annexure 4
- Label for Retention Sample : Annexure 5
- Sampled quantity for raw material (active) : Annexure 6
- Sampled quantity for raw material (inactive) : Annexure 7
- Label for ‘Sampled’ : Annexure 8
- Label for ‘UNDER TEST’ : Annexure 9
- Label for ‘Cleaned & Ready for Use : Annexure 10
- Format of Cleaning and usage log book for sampling devices : Annexure 11
- Label of Sample for Microbial Analysis : Annexure 12
- Label for Identification : Annexure 13
References (if any):
Reason for Revision:
- For better cGMP & cGLP
Abbreviation:
- 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
- SS sampling device : Stainless steel sampling device
- IPA : Isopropyl Alcohol
- cGMP : Current Good Manufacturing Practice
- cGLP : Current Good Laboratory Practice
Annexure 1
Raw material Control Register :
| Sr. No. | Date | Name of Material | Manufacturer / Supplier Name | GRN No. / Date | Batch No. / Lot No. | Mfg. Date | Exp. / Retest Date | Quantity Received | No. of Containers | A. R. No. | Worksheet No. | Quantity Sampled | Sampled By / Date | Date of Analysis | Date of Completion | Analyzed By | Status | Remarks |
Annexure 2
Sampling report of raw material :
| Sampling Report of Raw Material | ||
| 1 | Name of material / Item code : | |
| 2 | Name of Manufacturer / Supplier : | |
| 3 | GRN No. / Date : A. R. No.: | |
| 4 | No. of Containers Received : Total Quantity Received : | |
| 5 | Storage Condition : OK / Not OK | |
| 7. | Quarantine Label : a) Affixed b) Not affixed | |
| 8. | Packing | a) Drums / Bottles / Corrugated box |
| b) Fibre Plastic drums with polybag inside | ||
| c) PP woven bags with polybag inside / Paper bag with polybag inside | ||
| 9. | Packing condition: (OK / Not OK) (State observations if not satisfactory) | |
| 10. | Container Label Detail Verification | |
| a) Pharmacopeial Status (IP / BP / USP / EP / In-house) | ||
| b) Manufacturer’s Name | ||
| c) Batch No. / Lot No. | ||
| d) Batch Size | ||
| e) Date of Manufacturing | ||
| f) Date of Expiry / Retest | ||
| g) Storage Condition | ||
| h) Any other Remarks | ||
| 11. | Physical Appearance | |
| a) Presence of Lumps | ||
| b) Any abnormal odour | ||
| c) Heterogeneity between same container / container to container | ||
| d) Foreign Matter | ||
| e) Any other abnormality | ||
| 12. | No. of Containers Sampled : Sampled Quantity : | |
| 13. | Manufacturer’s Certificate of Analysis | |
| 14. | Remarks: | |
| 15. | Sampled By/Date: | |
Annexure 3
Sampling operational log book :
| Sr. No. | Name of Material | A.R. No. | Date of Sampling | RLAF Started at | Magnehelic Reading after 15 mins | Sampling Time | Sampling Done By | Remarks | |||
| Pre-Filter | Fine-Filter | Hepa-Filter | Start Time | End Time | |||||||
| 1 mm-5 mm | 5 mm-10 mm | 10 mm-20 mm | |||||||||
Annexure 4
Label of Sample for Analysis :
| Material name / Item Code____________________ GRN No. _____________ A.R. No._______________ Batch/Lot No. ___________ Batch size______________ Mfg. Date____________ Exp./Retest Date_________ Sampled _____________ Sampled by |
Quantity (Sign/Date)
Annexure 5
Label for Retention Sample :
| Material Name / Item Code____________________ GRN No. _____________ A.R. No._______________ Batch/Lot No. ___________ Batch size_____________ Mfg. Date____________ Exp./Retest Date_________ Sampled _____________ Sampled by Quantity (Sign/Date) |
Annexure 6
Sampled quantity for raw material (active) :
| Document No. | Page No. |
| Sr. No. | Material | Composite Sample Quantity (chemical + microbial analysis) | Sample Quantity for Retention | Sample Quantity for Microbial Analysis | Retest Sample Quantity | Sample Quantity for Identification (per sampled container) |
Annexure 7
Sampled quantity for raw material (inactive) :
| Document No. | Page No. |
| Sr. No. | Material | Composite Sample Quantity (chemical + microbial analysis) | Sample Quantity for Retention | Sample Quantity for Microbial Analysis | Retest Sample Quantity | Sample Quantity for Identification (per sampled container) |
Annexure 8
Label for ‘Sampled’ :
| SAMPLED Sampled by: (Sign. / Date) |
Annexure 9
Label for ‘UNDER TEST’ :
| UNDER TEST A.R.No.: Container No.: Sign./Date: |
Annexure 10
Label for ‘Cleaned & Ready for Use :
| CLEANED & READY FOR USE Sampling utensil : ID No. : Previous material : A.R. No. : Sign : Date : |
Annexur 11
Format of Cleaning and usage log book for sampling devices :
| Sr. No. | Date | Sampling devices | ID No.
| Used for Material | A.R. No. | Cleaning Time | Done By | Checked By | Remarks | |
| Started at | Completed at | |||||||||
Annexure 12
Label of Sample for Microbial Analysis :
| SAMPLE FOR MICROBIAL ANALYSIS Material Name / Item Code____________________ GRN No. _____________ A.R. No._______________ Batch/Lot No. ___________ Batch size_____________ Mfg. Date____________ Exp./Retest Date_________ Sampled _____________ Sampled by Quantity (Sign/Date) |
Annexure 13
Label for Identification :
| SAMPLE FOR IDENTIFICATION Material Name /Item Code_________________________ GRN No. _____________ Container No._______ ____ Batch/Lot No. ___________ A.R. No._______________ Mfg. Date____________ Batch size_____________ Sampled _____________ Exp./Retest Date_________ Quantity Sampled by______________ |
