by 1.0 OBJECTIVE
To lay down a procedure for performing, Sampling, Testing, Release and Retesting of Raw Materials.
2.0 SCOPE
This procedure is applicable for Sampling, Testing Release and Retesting of Raw Materials .
3.0 RESPONSIBILITY
Executive QC/officer QC : To conduct sampling, analysis and prepare coa of the material.
Section head : To ensure adherence to the requirements of this SOP and provide disposition of the material.
4.0 DISTRIBUTION
Master copy : Quality Assurance Department
Controlled copy – 1 : Quality Control Department
Controlled copy – 2 : Ware house
5.0 PROCEDURE
5.1 General instructions:
- Before sampling, QC executive/ officer QC shall check the following: Cleanliness of the sampling room, sampling booth, sampling utensils, raw material containers, packaging and storage condition of the raw material.
- In case of light sensitive material, sampling shall be performed under sodium lamp.
- Air supply in the sampling booth shall not be more than 25 mm/H2O and the return air shall not more than 7.5mm/H2O. Record in sampling room log book.
- Check the pressure differential of sampling room after every material sampling and record .
- Document details of the sampling activity in Sampling Room Log book.
5.2 Material Verification Before Sampling:
- QC Executive/ officer QC shall verify the number of containers received against the number mentioned in QC intimation slip for sampling.
- QC Executive/ officer QC shall verify that each container has a proper quarantine label.
- QC Executive/officer QC shall verify the manufacturer label on the container for its appropriateness.
- QC Executive/officer QC shall verify and match the information on the manufacturer label and quarantine label against the manufacturer’s COA and requisition slip, i.e. Batch. No., Mfg. Date, Exp Date, Manufacturer name, site address, etc.
- QC Executive shall verify the physical appearance of all containers to be sampled
- If any damage is observed to the container, resulting in exposure of raw material, QC Executive/ officer QC shall inform to QC head / Designee.
- QC head / Designee shall generate a rejection note and submit it to QA for further processing.
- QA personnel shall review the material and sign on the rejection note and document details in the respective log book.
5.3 Sampling plan
(A) For actives and Inactives
- QC Executive shall collect the sample as per the quantity mentioned in Annexure-7 for both chemical and microbial testing. This list shall be updated whenever a new material is included in the Site Portfolio.
- 100 % sampling shall be performed for all actives and inactives except for Vitamin D3.
- In case of Vitamin D3, sampling shall be performed from only one container chosen randomly per each consignment.
- If the consignment of sucrose is received in more than 50 containers / packets per batch, then sampling shall performed as per √ N+1 criteria.
- For active and inactive raw materials, sample shall be collected from all containers for identification in separate individual polythene bags labeled with AR no, and container no. In addition, sample shall be collected from each container in a separate polythene bag to make the composite sample. For every batch, two composite samples shall be prepared. i.e. one for analysis labeled and another for control sample labeled .
(B) Sampling Procedure:
- Raw Material In-charge shall receive two copies of “QC Intimation for Sampling” from Raw material store. Before initiating the sampling activity QC exective/officer will fill the initial part i.e. Material name, Item code, COS grade and form details of the received material. In case a CEP material received, review the vendor coa for the CEP No of the material. If the CEP No.is not available inform procurement to obtain the coa including the CEP No. Compare the CEP No. on the COA against the no. available on the EDQM website. If the numbers match proceed with the sampling process However it there in a mismatch identified in the number, report the matter to procurement and discontinue the sampling.
- Before proceeding the sampling, QC Executive/ QC officer shall enter details about the material from the QC Intimation slip for Sampling, Raw material Inward register and generate an A.R No through ERP and record it , Raw Material Inward Register and on the QC Intimation slip for sampling.
- QC Executive/QC officer shall follow SOP No. QC/267 for gowning procedure during sampling.
- Before proceeding for sampling, switch on the RLAF and wait for 30 minutes to allow the RLAF to stabilize. Record the magnetic gauge reading , Sampling Room Log book.
- QC executive/ QC officer shall sanitize hands with IPA solution and wear gloves, head cover, and other safety garments. he/she shall again sanitize hands before handling any material/container/bag.
- As a part of sampling, the sampling personnel shall confirm that the material is received from the approved site of an approved manufacturer from the manufacturer’s certificate of analysis to ensure that the indented material is received correctly.
- During sampling, analyst shall check, Packaging condition, Labeling requirements and any other exclusive requirements of the material container.
- QC Executive/QC officer shall record all relevent details , Raw Material Sampling Report.
- QC Executive/QC officer shall verify the cleanliness of containers and sampling tools, Before performing the sampling.
- Material container/bags shall be opened inside the sampling booth and sampled carefully by QC executive/QC officer using sampling rod or appropriate tools. Sample shall be collected from Top, middle and bottom of each container.
- QC Executive/QC officer shall collect the sample in polythene bags and affix label , sampled label.( on the sampled container)
- For Microbial analysis, sample shall be collected in a sterile container and the container shall be tightly closed after sampling.
- QC executive shall bring all the sampled material to the lab for analysis.
- Upon completion of sampling, the container shall be closed tightly and a sampled label shall be affixed on the containers/bags , sampled label.
- QC Executive shall fill all details of sampling , Raw Material Sampling Report.
- Clean the sampling room (cleaning procedure for sampling room) and sampling tools (identification and cleaning of raw material sampling tools).
- QC Executive shall dispose the gloves, mask, head cover and shoe cover in waste bin.outside the sampling booth
5.4 Testing of samples:
- The test for infrared spectroscopy (IR) shall be mandatorily performed as the identification test if it is included in the specifications.
- If IR spectroscopy is not included as an identity test, any single identification test shall be performed on all the containers of the consignment.
- In case of inactives, if there is no identification test in the specification, the test for description will be accepted as the identification test.
5.5 Testing
- Section in charge/designee shall plan the testing of the sampled raw materials.
- Section in charge/designee shall allot the sample to the qualified analyst along with QC Intimation slip for sampling, specification, standard test procedure and analytical data sheet for analysis.
- Section in charge/designee shall submit the sample requiring microbial analysis to the microbiology section.
- QC analyst shall perform the testing as per respective approved test procedure and record results in the analytical data sheet.
- For identification by IR, in the case of non-availability of working/reference standard, previously approved material shall be used as the standard.
- After completion of testing, QC analyst shall submit the analytical data sheet along with all the meta data to the reviewer. If any discrepancy is found during the review of the raw material testing data, inform to head QC/designee to adopt appropriate QMS tools for investigation.
- Reviewer shall review all the raw data, weight slips analytical data sheets, Microbiological test report, audit trial data and electronic data and submit the data for approval to section head/designee.
5.6 Disposition of raw material
- Section head / designee shall decide the disposition of the material as per the data obtained in the analytical raw data sheet.
- On approval, QC executive/QC officer shall enter results obtained for the material in ERP and the section head shall authorize /release the material in ERP. QC executive/QC officer shall generate the COA and attached with the data sheet.in case Reject the material inform to QC Head and follow QAMS tools.
- After authorization by Q.C. personnel, Approved/Rejected label as appropriate shall be affixed on each container or bag in the raw material store in such a manner that the term “Quarantine” is covered on the Quarantine label and all other information is easily visible.
5.7 Re-testing
- The purpose of assigning a retest date to any material is to test the material based on the in-house procedure and/or manufacturer recommendation, thereby assuring that the material being stored at specified storage conditions meets approved specifications at all times before its usage.
- Expiry date: It is the date beyond which a material cannot be used and is the maximum validity for that material, based on the manufacturer’s certificate of analysis or packaging label of the material mentioning the specific term “Expiry”.
5.8 Retest:
- It is the date beyond which the material cannot be used without re-testing unless the material has already expired.
- Whenever the manufacturer claims that the material is to be re-evaluated after a certain date, consider the date/interval, it is less than the re-testing date mentioned in the sop. If it is at a date later than the period mentioned by this SOP, follow this SOP for assigning a new re-testing date.
- In the event the manufacturer provides an expiry date, retest period shall be as follows In the event the RM is provided a retest date approach the manufacturer for stability data to extend the shelf life of the material basis which a retest shall be conducted . Active raw materials 1 year from initial date of release
- In-actives 2 years from initial date of release (include solvents, flavors).
- Enzymes and vitamins: 6 months from initial date of release.
- Based on the terms used by the manufacturer, if it does not imply expiry date, it shall be taken as re-test date.
- Re-testing shall be continued up to expiry data provided by manufacturer or 5 years from the date of manufacturing expiry whichever is earlier.
5.9 Sampling procedure for retesting :
- For raw materials under retest, sampling shall be performed as per above mentioned sampling procedure and collected from each available container in a polythene bag to make the composite sample.
- Re-test sample shall be labeled as per , retest sampled label. After sampling, relevant details shall be documented in , “Raw Material Retest Inward Register”.
- For re-test materials, following tests shall be performed.
- Description of the material (Physical appearance)
- Assay
- Chromatographic impurities or related impurities (if applicable)
- Loss on drying / Water content.
- Microbial limit test. (If applicable)
- After analysis, if the material is approved, affix the Re-test approved label .
- If the material does not meet the specifications, investigate through OOS procedure or other QMS tools.
6.0 ABBREVIATIONS
QC – Quality Control
Qty. – Quantity
SS – Stainless Steel
GRN No. – Goods Receipt Note No.
B. No. – Batch Number
Mfg. – Manufacturing
Exp. – Expiry
ERP – Enterprise Resource Planning.
COA – Certificate of Analysis.
QMS – Quality management system.
OOS – Out of specification
No. – Number
CEP – Certificate of suitability
EDQM – European Directorate for the Quality of Medicines and HealthCare
