| Sampling of Raw material |
1.0 OBJECTIVE To lay down a procedure for Sampling of Raw Material. 2.0 SCOPE This SOP is applicable for Sampling of Raw Material for microbiological and chemical analysis in Quality Control Department. 3.0 RESPONSIBILITY QC officer/ Sr. officer/ Executive / Sr. Executive 4.0 ACCOUNTABILITY Head-QC 5.0 PROCEDURE 5.1 Physical checks before sampling: 5.1.1 Check the vendor list to ensure that the material is from approved vendor. If the material received from Non-approved vendor, then sampling shall not be done and then inform to head QC. 5.1.2 If the COA of the raw material is not received, then inform to head QC, after approval from head QC, sampling shall be done. 5.1.3 Check the physical status of the container/bags and make entries in “Inspection report for raw material” (as mentioned in format number XXX. 5.1.4 Check the packing conditions of container/bags/packs for any damage. 5.1.5 Information shall be given to the Head QC for any container/bag found physically damaged or found without seal. QC head will inspect the container/bag for intactness of innermost packing. 5.1.6 The rejected label shall be affixed on the rejected container/bag. 5.1.7 Based on sampling plan, prepare sample for analysis label, control sample, under test label). 5.1.8 Record the entries of raw material sampled, in “Sample Quantity List of raw material” 5.2 Sampling of Sterile Raw material (Dry Powder for Injection) with Satellite sample 5.2.1 Every sterile raw material shall be received with a satellite sample which is the representative sample of entire received lot of Raw Material. 5.2.2 Satellite samples are the composite sample of entire lot of sterile Raw Material collected aseptically from every container during the filling process by the Raw material manufacturer. 5.2.3 After receiving the sterile Raw Material in store, warehouse person will inform to Micro department. 5.2.4 Microbiologist will receive the GRN along with certificate of analysis of material from the warehouse person. 5.2.5 From the received GRN, enter the details as per format number “Raw Material Inward Register”. 5.2.6 The microbiologist shall collect the satellite sample from store department and put it into the sanitized SS- canister and take it to the microbiology laboratory. 5.2.7 This Satellite sample then transferred to the sterility room as per the procedure defined in respective SOP for the Sterility testing and BET testing. 5.2.8 After taking the sample for sterility testing, BET testing and the left-over sample shall be transferred to the QC laboratory for the chemical analysis. 5.2.9 The sampling of control sample shall be done at the time of dispensing of material. 5.2.10 The Quantity of Control Sample shall be taken twice then that of Micro & Chemical sample. 5.3 Sampling of Sterile Raw material (Dry Powder for Injection) if Satellite sample not received 5.3.1 In-case if the satellite sample is not available with the sterile raw material, sampling of the raw material shall be done in dispensing area. 5.3.2 Only trained Microbiologist are responsible for the sterile raw material sampling. 5.3.3 All tools used for sampling of sterile raw material should be properly cleaned and dehydrogenated as per the respective procedure. Sampling tool detail is mentioned below: 5.3.3.1 SS-Spatula: For sample collection 5.3.3.2 SS Scissor: To break the aluminum seal 5.3.3.3 Sterile Container (about 100 ml Capacity) for the sample collection for sterility and Chemical analysis 5.3.3.4 Sterile Container (about 100 ml Capacity) for the retention sample 5.3.3.5 Dehydrogenated container (about 10 ml capacity) for BET testing 5.3.4 Microbiologist shall carry the dehydrogenated sampling tools in sanitize (by 70% IPA Solution) SS container to the store department. 5.3.5 Follow the procedure of entry and exit in RM store as per the respective SOP. 5.3.6 Collect the GRN from the store person and enter the detail of consignment (Raw Material) in the Inspection Report of the Raw Material 5.3.7 Physically inspect each container of the received consignment and if any defect and abnormality found in the container, mention in the Inspection Report. Do not do the sampling if the container found damaged or seems the integrity of the material may be affected due to any reason. Immediately inform the matter to QA department for the further action. 5.3.8 Verify the details (as mentioned below) of raw material received against GRN. 5.3.8.1 Name of the material & Pharmacopoeia status 5.3.8.2 Material code 5.3.8.3 Batch No. 5.3.8.4 Quantity received 5.3.8.5 Mfg. date / Expiry date 5.3.8.6 Vendor COA 5.3.8.7 Quarantine label affixed by warehouse etc. 5.3.8.8 Mfg. site address on COA, material label and AVL. 5.3.9 Cross check the material information mentioned on container label with GRN. 5.4 Transfer of Raw Material containers to Dispensing Area 5.4.1 Sanitize each container with 70% IPA solution and then place it into the pass box along with SS container of sampling tools. Let it outer surface get sanitize by the UV light for at least 10 minutes. 5.4.2 Now enter to the dispensing room by following the procedure of entry and exit as mentioned in respective SOP. 5.4.3 Ensure the area is cleaned and free from any previous material. Now check the temperature and humidity of the area which should meet the acceptable limit (Temperature 23±20C and Humidity not more than 50%). 5.4.4 Now transfer the RM containers to the Dispensing RLAF (Reverse Laminar Air Flow) and put it on the SS table provided in the RLAF. 5.4.5 Note: At the end of cleaning, Microbiologist shall inspect the area and make a record of it in the “RLAF Sequential log for usage and cleaning” as per format number. 5.4.6 Again sanitize the container with 70% IPA solution and now break the seal of lid with help of dehydrogenated scissor and open the lid carefully. 5.4.7 Collect the required quantity of the sample in first sterile container for sterility/chemical analysis, and retention sample in second sterile container and for BET transfer the required sample quantity in dehydrogenated glass tube. 5.4.8 Composite sample shall be prepared by collecting. 5.4.9 Mention the required information on the label of container for proper identification. 5.4.10 Carefully close the container lid in aseptic conditions to avoid any accidental contamination during the sampling procedure. Put the raw material sample container in SS canister. 5.4.11 Clean the working area if any material spillage is there with 70% IPA solution. 5.5 Sample transfer to Microbiology laboratory 5.5.1 After completion of Raw material sampling, take back all the sampled raw material container to the Approved RM store through the pass box including the Raw material sample containers. 5.5.2 Put back the sampled container at its designated place. 5.5.3 Transfer the SS container having raw material sample bottles to the microbiology laboratory for analysis. The sample collected for retention sample shall be handed over to QA department. 5.5.4 Note: The sample collected in dehydrogenated container shall be used for BET testing and other bottle of shall be used for the sterility testing under the LAF. After performing the sterility test the leftover sample shall be transferred to the QC lab for chemical analysis. 5.6 Sampling tools: 5.6.1 Sampling tools to sample different type of raw materials, shall be as mentioned below: 5.6.1.1 Spatula – For sampling of material from small solid bulk container/bags. 5.6.1.2 SS sampling rod – For sampling of solid raw materials from bags/drums. 5.6.2 Use always clean dry bottles with screw caps for collecting liquid samples and fresh poly bags/dry bottles for solids. 5.6.3 In case of light sensitive materials use black poly bags or amber bottles for sampling. 5.6.4 Use cleaned and dried set of sampling equipment’s for each item while sampling. 5.7 Sampling Plan: 5.7.1 For active material: The sampling following active raw material shall be done from all received container/bags (100%). 5.7.2 For excipients: If container/bags are 4 or less, carry out sampling from all the container/bags (100%). If container/bags are more then 4, follow √n + 1method for sampling. For example, – (a) For 5 containers-√5+1= (2.24+1) = 3.24 ≈ 3 container out of 5 is to be sampled. (b) For 8 containers-√8+1= (2.83+1) = 3.83 ≈ 4 container out of 8 is to be sampled. 6.0 ABBREVIATIONS SOP – Standard Operating Procedure QC – Quality control RLAF – Reverse laminar air flow RH – Relative humidity GRN – Goods receipt note BET – Bacterial Endotoxin Limit IPA – Isopropyl alcohol UV – Ultra violet |