Follow
OBJECTIVE : To set up a procedure for testing and release of raw materials for manufacturing of products.
SCOPE : This procedure is applicable for testing and release / rejection of raw materials in the quality control laboratory of (Company Name).
RESPONSIBILITY :
1. QC Analyst/ Officer shall be responsible to perform the activity as per procedure.
2. Sr. Officer / Asstt. Manager QC shall be responsible to ensure proper and timely execution of procedure.
3. Manager QC or designee shall be responsible for effective implementation and training of procedure.
PRECAUTIONS :
1. Ensure that the analyst is following the current specification and standard testing procedure (STP) which is prepared based on the current edition of the Pharmacopoeia / regulatory requirement.
2. Check the calibration status of instruments to be used and ensure validity.
3. Check validity of working/reference standard to be used for analysis.
PROCEDURE :
– Ensure proper cleaning of working table before and after the analysis.
– Check whether sampling was performed as per sampling procedure mentioned in SOP.
– Follow the flow chart given in Annexure –I for approval or rejection of raw material after analysis.
– Review the raw material register (Annexure II), collect the raw material sampling sheet, certificate of analysis from supplier (if available) along with sample.Check details of label on samples and match with those on raw material sampling sheet and certificate of analysis from the supplier (if available).
– Test the material as per the approved STP of respective raw material and record the result in analytical report sheet / worksheet.
– Mention the AR No. allotted to the sample in the AR register on the composite sample label before start of analysis. For active raw materials (API) having more than one identification test including IR, perform the identification test by IR for each individual container and the other identification tests on composite samples.
– If Identification test by IR is not available for a raw material, then perform the chemical/physical identification tests for each individual container.
– Upon confirming the identification of all containers, perform other tests on composite samples.
– If any specific test for which in-house facility is not available, send the material to approved outside testing Laboratory (Contract Laboratory) along with the approved specification and STP (only the relevant part). The contract laboratory will perform the test (s) as per the approved STP provided by Beximco and share the report. The details of samples sent shall be recorded in FRM No.: FQC/537 (Annexure- VI).
– The analytical report received from outside testing laboratory shall be reviewed by manager QC or designee. The concerned batch shall be released or rejected only after receipt and review of the test report received from outside testing laboratory.
– However, in case it takes a longer time to receive the test report (s) from the contract laboratory, the batch may be released to continue finished product manufacturing based on the data provided by the supplier in their Certificate of Analysis. This shall be done taking appropriate deviation as per SOP No. QA008.
– If the test report received from the contract laboratory indicates that the sample fails to meet Beximco specification, the concerned batch of the material as well as the product manufactured using the material will be rejected.
– Perform the Residual Solvent test initially on the first 3 consecutive batches/lots of any material from a specific supplier followed by one batch / lot per year.
– After completion of full testing on at least 3 batches / lots for a raw material and 3 batches/lots of excipients, reduced testing of the material from a specific supplier shall be done. In this case, identification and critical tests mentioned below, must be done on each batch/lot and data of the other parameters shall be taken from the supplier’s
certificate of analysis. However, perform full testing on every 10th batch/lot or one batch per year whichever comes first.
Critical test: Would include appearance, assay, related substances (API only), water content/LOD, Bulk/Tapped density etc.
Non-critical test: Would include ash / sulphated ash, heavy metals, absorbance of solution, acidity or alkalinity, water / ether soluble substances etc.
– Any reduced testing plan that is applied to material for products being exported must be accepted by the customer. In the event of the reduced testing plan not being accepted by customer performs the full testing for every batch.
– In case of reduced testing, if any batch of a material fails to meet any of the critical parameters, reject the batch and follow full testing from the next batch which shall be continued for the next 3 batches / lots for an API and 3 batches / lots for an excipient.
– If a quantity of excipient that was fully tested and released earlier is received as a separate consignment as a new MRR, perform only identification test on all containers under the new MRR.
– Prepare the analytical report for the material as per respective approved raw material specifications. The Analytical report sheet (Analytical Worksheet) is a preprinted approved format, consisting of all tests which is preferably material/product specific and is always in line with the current approved specification/STP.
– Prior to making entries in the Analytical Report sheet, perform the `calculation of results like Assay by HPLC, Related Substances by HPLC, Residual solvents by GC etc. using test specific Microsoft excel worksheets which are prepared, validated and processed following the approved STP.
– Ensure the security of excel worksheets through password protection of the output and non-input cells along with controlled access to users.
– Complete the analysis of raw materials within six weeks from the date of sampling. If analysis of a material is not possible to be completed within six weeks of
sampling raise a deviation to justify the delay with proper investigation.
– Discuss any specific non-conformance (OOS) / OOT situation with Quality Control Manager/in-charge and follow the relevant SOP for handling of OOS/ OOT results.
– On completion of analysis, as per the approved specification and STP, the completed analytical report (certificate of analysis and records of analysis) must be reviewed by two senior QC personnel (Sr. officer/ Manager) before QC approval.
– In cases, where there is an urgent requirement of using excipients for production to ensure product supply to the market, release excipients requiring microbiological test for use only after full chemical test.
However, complete the microbiological test and ensure data is ready before releasing the finished product to the market. This situation is applicable only for the finished products to local market.
– QC Analyst / Officer shall enter Assay, LOD/Water/ (Water + Organic Solvents) for all active materials in the inventory management system (if applicable).
– Release the material, in case it conforms to specification, and if not, it shall be rejected in the system by Manager QC/ designee. In case of transit damage to the container (when the chemical nature of the material is not changed) the material may be partly released and partly rejected in the system, depending on its quality status.
– Take print out of RELEASED /REJECTED labels for each container of the material with one additional label and sign the same (Annexure–III /IV). The additional copy of the RELEASED /REJECTED label shall be affixed with the analytical dossier.
Include the value for assay, LOD/Water on the released label for API.
– Send duly signed copies of Material Receiving Report (MRR) (Original, Second and Third copy) along with the Certificate of Analysis (COA) to warehouse and retain the fourth copy with the analytical dossier.
– Cross-check the information of the “Released/Rejected” label with that of the Supplier’s label as well as of the quarantine label. Affix the labels in such a way that it covers all the previous information, e.g. quarantine label, sampled label.
– Affix the “Released/ Rejected” label in cascading manner of the respective containers in presence of Warehouse personnel. Ensure to cross out the manufacturer/supplier released label before affixing the released label.
– QC Analyst / Officer shall file the certificate of analysis, records of analysis, supplier’s certificate of analysis (if available), microbiology reports (if applicable) chronologically as per internal AR. No. Completed report shall be filed in raw material report file and stored in documentation cell.
– In case of rejection of material, send the copy of certificate of analysis along with raw material rejection memo as per Annexure-V to Warehouse Manager.
– Before release/rejection of a batch of raw material, record the discrepancies (if any) in Annexure-VI of (FRM No.: FQC/303). Deviations can be observed as under:
– During visual inspection (e.g., container closure system, labeling, supplier CoA, etc.),
– During sampling (e.g., appearance of material, foreign particles, etc.), and
– During analysis (e.g., out of specification, out of trend results, etc.).
– In case the computer system is not in operation because of some unavoidable circumstances, the total system starting from sampling, release/rejection and labeling shall be performed manually.
– Dispose the remaining quantity of raw material samples as per procedure of disposal of reminder sample.
