SOP for receipt and storage of Samples in Quality Control Laboratory – Raw Materials, Semi – Finished, Finished Products and Packaging Materials in Quality Control Laboratory
1.0 Purpose:
To lay down a procedure for Receipt of Raw Materials, Semi-Finished (Bulk finished), Finished Products and Packaging Materials in Quality Control Laboratory.
2.0 Scope:
The scope of this SOP is applicable for Receipt of Raw Materials, Semi – Finished, Finished Products and Packaging Materials in Quality Control Laboratory. This SOP also applies for the procedure for Analysis of Semi-Finished (Examples – Granules, Blend, Pellets, Compressed Tablet, Coated Tablet, Filled Capsules, Before Filtration Sterile Product and After Filtration Sterile Product) and Finished Products.
3.0 Responsibility:
3.1 QC-Personnel (Analyst): Analysis & Data Entry in LIMS.
3.2 Lab QA reviewer: To review the data in LIMS.
3.3 Supervisor QC/Section In-charge:
To receive the SFG/FG/PM and RM samples.
Sample discard in LIMS:
3.4 Head QC/Designee:
To review the data in LIMS.
Approval of RM and PM in LIMS
3.5 QA Personnel: Approval of semi-finished and finished product in LIMS.
3.6 IPQA Personnel: To perform the sampling activity of semi-finished & finished product.
4.0 Definitions:
Not applicable
5.0 Procedure:
5.1 Following stages is defined as Semi-Finished Products :
- Granules.
- Blend and Pellets.
- Compressed Tablets.
- Coated Tablets.
- Filled Capsules.
- Before Filtration Sterile Product.
- After Filtration Sterile Product.
5.2 Completely packed product is termed as finished product.
5.3 Sterile products sealed in its primary packaging material shall be considered as finished product for analysis.
5.4 All analytical samples shall be analyzed as per respective specification in the Quality Control laboratory.
5.5 During analysis, in case any handling loss of tablet, capsule and injectable samples occurs, it need to be justified with proper remark and authorization from Section In-Charge in LIMS.
5.6 Store the samples as per the storage conditions mentioned in the specification.
5.7 Procedure for Semi-finished and finished Inward:
5.7.1 QA (IPQA) person shall carry out the sampling activity of semi-finished and finished product as per “SOP for Sampling and Release of Semi-Finished Product” and “SOP for Sampling of Finished Product”.
5.7.2 QC person shall receive the sample from IPQA personnel. He/ She shall verify following details in LIMS.
- Sample Number
- A.R. No.
- Product Name
- Stage
- Batch No.
- Sampled Quantity
- Date of Sampling
- Sampled By
- Storage Temperature
5.7.3 QC Personnel shall verify the sample label at the time of sample receipt.
5.7.4 QC person shall keep the samples in respective sample storage cabinet, as per their storage condition.
5.7.5 Section in – charge/Designee shall allocate the work to analyst in LIMS and handover the sample to analyst for analysis in LIMS as per “SOP for Lot Management in LIMS”.
5.7.6 During receipt of sample for analysis analyst shall verify all the details on sample label and ensure correctness of samples in LIMS. There after analyst shall perform the analysis as per the respective specifications.
5.7.7 Supervisor-QC/ Section In-charge shall prepare the composite sample for the defined test (like Assay, Content Uniformity, Dissolution, Related substance, etc.) wherever sample received from start, middle and end of the manufacturing process.
Note: In case of individual tablets / capsules to be used for analysis e.g. Dissolution, Content Uniformity, tablet order to be used in test is in ascending order with respect to start, middle and end. Like in case of dissolution test (On 6 tablets), first 2 tablets to be taken from “Start” sample, other 2 tablets from “Middle” sample and remaining 2 tablets from “End” sample.
5.7.8 For coated tablets, Supervisor-QC/ Section In-charge shall prepare the composite sample for the defined test (like Assay, Content Uniformity, Dissolution, Related substance, etc.) from each lot.
5.7.9 Analyst shall perform the analysis and update the data in LIMS.
5.7.10 Lab-QA Reviewer shall review all the data in LIMS.
5.7.11 Head QC or designee shall give the final approval of RM & PM in LIMS.
5.7.12 Lab-QA/ IPQA person shall give the final approval of semi-finished and finished product in LIMS.
5.7.13 In certificate of analysis (CoA) of the semi-finished Product the following details shall be provided;
- Product Name
- Product Code
- Specification Id.
- Batch No.
- Mfg. Date
- Sampled By
- Sampling Quantity
- Batch Size
- Specification Rev. No.
- A.R. No.
- Exp. Date
- Sampled On
- Retest Date
- Test
- Result
- Standard
- Analyzed By
- Checked By
- Approved By
5.7.14 In certificate of analysis (CoA) of the finished product the following details shall be provided;
- Product Name
- Product Code
- Specification Id.
- Batch No.
- Mfg. Date
- Pack Style
- Inspection Lot No.
- Specification Rev No.
- A.R. No.
- Exp. Date
- Quantity Packed
- Test
- Result
- Standard
- Analyzed By
- Checked By
- Approved By
- In certificate of analysis (CoA) of the Raw Material the following details shall be provided:
- Material Name
- Material Code
- Specification Id.
- Control No.
- Mfg. Date
- Mfg. Batch No
- Packing Type
- Quantity Received
- Inspection Lot No.
- Specification Rev. No.
- A. R. No.
- Exp. Date
- Manufactured By
- Retest Date
- Date of release
- Test
- Result
- Standard
- Analyzed By
- Checked By
- Approved By
5.8 Procedure for Raw material Sample inward:
5.8.1 After sampling of raw material, sampler carries the sample along with vendor CoA, to Quality Control Laboratory and hand over the sample to QC Personnel / Section In-charge.
5.8.2 QC-Personnel shall verify the all required details in LIMS as mentioned below;
- Sample name
- Material Code
- Inspection Lot No.
- A. R. No.
- Mfg. Date
- Exp. Date
- Mfg. Batch No.
- Manufactured By
- Quantity Received
5.8.3 Sample is stored in the “Sample Storage Cabinet” as per their respective storage conditions in Quality Control Laboratory and the Control Sample is transferred to the Control Sample Room and is handled as per SOP for “Collection, Storage and Disposal of Control Sample (Reserve Sample) of Raw Material and Finished Product”. .
5.8.4 Further Sample is allocated for analysis. For Analysis and release procedure refer SOP for Analysis and Release of Raw material.
5.9 Procedure for Packaging material Sample inward:
5.9.1 After sampling of Packaging Materials, sampler carries the sample along with vendor CoA, to Quality Control Laboratory and hand over the sample to QC Personnel / Section In-charge.
5.9.2 QC-Personnel shall verify the all required details in LIMS as mentioned below:
- Sample Number
- A.R. No.
- Material Name
- Supplier Lot No.
- Control No.
- Sampled Quantity
- Mfg. Date
- Exp. Date
- Date of Sampling
- Sampled By
5.9.3 After verification of above details supervisor-QC/Section In-Charge receive the sample in LIMS through Sample Number.
5.9.4 Sample is stored in the “Sample Storage Cabinet” in Quality Control Laboratory.
5.9.5 Further Sample is allocated for analysis. For Analysis and release procedure refer SOP for Analysis and Release of Packaging material.
5.10 Procedure for Sample Discard:
5.10.1 Supervisor-QC/ Section In-Charge shall physically verify the available quantity (Balance Quantity) against the quantity show in LIMS.
5.10.2 After completion of all analysis and review activity, Supervisor-QC/ Section In-charge shall discard the sample as per SOP for Standard Operating Procedure for Disposal of Left Over Sample and Scrap, and update details in LIMS.
5.10.3 Flow the sample for destruction in LIMS;
5.11 Storage of under test samples in Quality Control Laboratory:
5.11.1 All Under Test Samples shall be kept in the respective cabinets under lock and key.
5.11.2 Sterile/Injectable Material Products shall be stored as per the product storage condition or as mentioned in the respective specification, in the cooling cabinet/Deep freezer at ambient temperature.
5.11.3 For cold chain product (2°C – 8°C / – 20 °C), maintain the product / material list as per Format, “Format for storage condition of cold chain product / raw material”.
5.11.4 In case of cold chain product (i.e. 2°C – 8°C / – 20 °C) mentioned as per respective Format, carry the sample from stability chamber to Quality Control Laboratory in container with cool pack container.
5.11.5 Cabinets for storage of Under Test samples shall be separate for Active Raw Material, Excipient and Liquid Samples.
5.11.6 Semi – Finished and Finished Product shall also have separate Cabinets for Storage.
5.11.7 Raw material Liquid under Test sample shall be stored in a separate Storage Cabinet.
5.11.8 Stability Study Sample shall be collected and stored separately as per the storage condition.
5.11.9 Always handle the under test samples carefully.
5.11.10 Avoid spillage and contamination while handling the under test samples.
5.11.11 Wear Personal Protective Equipment (PPE’s) like Hand Gloves, Safety Goggles, Nose Mask (Whichever applicable) while handling under test samples.
5.11.12 Sample Storage Cabinets are placed in the Quality Control Laboratory.
5.11.13 Section In charge/Designee shall allocate the under test samples for Analysis as per “SOP for Lot Management work flow in LIMS”.
5.11.14 In case the analysis is pending or not completed, the under test sample shall be kept in the respective storage cabinet.
5.11.15 After the completion of Analysis, Reviewer shall review the data in LIMS.
5.11.16 For Raw Material, Finished Product, Stability and Process Validation sample shall store as per the respective Format.
5.11.17 The Temperature of the Quality Control Laboratory shall be about below 25 ºC except for Hot Room.
5.11.18 In case of LIMS breakdown, entry shall be done in the logbooks provided as per the SOP. On restoration of system, data shall be inward into the LIMS.
6.0 Frequency:
As and when required for semi-finished, finished products and raw materials.
7.0 Format for recording:
- Semi – Finished (Blend) Inward Register
- Semi – Finished (Core) Inward Register
- Semi – Finished (Coated) Inward Register
- Process Validation Inward Register (Intermediate sample)
- Finished Product Inward Register
- Approved Stamp
- Rejected Stamp
- Cleaning Validation Inward Register
- Innovator Sample Inward Register
- Innovator Sample Consumption Record
- Hold time Study Sample Inward Register
- Raw material Sample Inward Register
- Distribution list of SOPs and Formats/Annexures
- Format for “Raw Material, Finished Product, Stability and Process Validation Sample Storage cabinet.
- Format for Storage Condition of cold chain product/ raw material.
7.1 Format for Semi – Finished (Blend) Inward Register
Receipt Date
Product Name
Batch No.
Mfg. Date
Exp. Date
Batch Size
Qty. Sampled
Sampled By
Storage condition
Sample Storage at respective condition (Yes/No)
A.R.No.
Recorded By
Sign & Date
Release Date
Analyst
Leftover Sample Destroyed By
Verify By
Remarks
7.2 Format for Semi – Finished (Core) Inward Register
Receipt Date
Product Name
Batch No.
Mfg. Date
Exp. Date
Batch Size
Sample Quantity Received
Sampled By
Storage condition
Sample Storage at respective condition (Yes/ No)
A.R. No.
Recorded By
Sign & Date
Release Date
Analyst
Left over Sample quantity destroyed after analysis
Leftover Sample Destroyed By
Verified By
Remarks
7.3 Format for Semi – Finished (Coated) Inward Register
Receipt Date
Product Name
Batch No.
Mfg. Date
Exp. Date
Batch Size
Sample Quantity Received
Sampled By
Storage condition
Sample Storage at respective condition (Yes/ No)
A.R. No.
Recorded By
Sign & Date
Release Date
Analyst
Left over Sample quantity destroyed after analysis
Leftover Sample Destroyed By
Verified By
Remarks
7.4 Format for Process Validation Inward Register (Intermediate sample)
Receipt Date
Product Name
Batch No.
Mfg. Date
Exp. Date
Batch Size
Sample Quantity Received
Sampled By
Storage condition
Sample Storage at respective condition (Yes/ No)
A.R. No.
Recorded By
Sign & Date
Release Date
Analyst
Left over Sample quantity destroyed after analysis
Leftover Sample Destroyed By
Verified By
Remarks
7.5 Format for Finished product Inward Register
Receipt Date
Product Name
Batch No.
Mfg. Date
Exp. Date
Batch Size
Sample Quantity Received
Sampled By
Storage condition
Sample Storage at respective condition (Yes/ No)
A.R. No.
Recorded By
Sign & Date
Release Date
Analyst
Left over Sample quantity destroyed after analysis
Leftover Sample Destroyed By
Verified By
Remarks
7.6 Format for Cleaning validation sample Inward Register
Receipt Date
Previous Product
Active to be Tested
Equipment Name
A.R. No.
Batch No.
Storage Condition
Sample Storage at respective Condition (Yes/ No)
Recorded By Sign & Date
Release Date
Analyst
Leftover Sample Destroyed By
Verify By
Remarks
7.7 Innovator Sample Inward Register
Sr. No.
Product Name
Manufacture
Batch No.
Mfg. Date
Expiry Date
Storage condition
Sample Storage at respective condition (Yes/ No)
Sample Received From
Sample Received by
Sample Quantity Received
A.R. No.
Recorded By Sign & Date
Remarks
7.8 Innovator Sample Consumption Record
Sr. No.
Recorded By Sign & Date
Date of Receipt
Batch Number
Mfg. Date
Exp. Date
Quantity Received
Quantity Consumed
Balance Quantity
Purpose
Date of Use
Analyzed by
Checked by
Remarks
7.9 Hold time Study Sample Inward Register
Receipt Date
Product Name
Batch No.
Mfg. Date
Exp. Date
Batch Size
Stage
Sample Quantity Received
Storage condition
Sample Storage at respective condition (Yes/ No)
A.R. No.
Recorded By Sign & Date
Release Date
Analyst Left over Sample quantity destroyed after analysis
Leftover Sample Destroyed By
Verify By
Remarks
7.10 Format for storage condition of cold chain product / raw material
Storage condition list of cold chain product / raw material
| Sr. No | Name of the Product / Material | Storage Condition | Updated by |
| Note: List is applicable for cold chain material (2-8°C / – 20 °C), Other materials / products to be stored at NMT 25 °C. |
| Prepared By: Sign & Date | Checked By: Sign & Date | Approved By: Sign & Date |