LAB-100 Laboratory In Process and Finished Product Quality Control

5.1    Receiving Samples in the QC Laboratory

5.1.1 Production personnel should deliver the sample to the QC laboratory sample booth, log the sample into Logbook Bulk and In-Process Sample Logbook, sign the Logbook and enter the required information as specified by the Logbook.

5.1.2 Upon receipt in the Laboratory, the Laboratory Administrator or designee should check the sample labels against the entry in the Logbook.

5.1.2.1 If the information on the label matches the entry in the Logbook, the

Laboratory Administrator or designee sign off in the Logbook and the sample is logged into the Finished Goods database.

5.1.2.2 If the information on the label does not match the entry in the Logbook, the Laboratory Administrator or designee must notify the Laboratory Manager that the sample is not accepted in the Laboratory.

5.1.3 The sample should then be transferred to a designated area within the Laboratory.

5.2    Scheduling Test

5.2.1 The Laboratory Manager or designee needs to make sure to schedule work according to priority list provided by the marketing and supply. Otherwise samples should be tested on a first in first out basis.

5.2.2 Sample turnaround times are indicated below:

5.2.2.1 In-Process Blends, Bulk Capsules, Bulk Tablets (end of run/coated), Finished Liquid – 10 days from receipt.

5.2.2.2 In-Process tests – as soon as received (maximum 1 day).

5.2.3 Where microbiological testing is required, the microbiological samples are to be submitted to internal or external microbiology laboratory.

5.3    Testing and Reporting

Upon receipt of the sample for testing, the Laboratory Analyst must:

5.3.1 In the Finished products database:  Change status from “logged in” to “under test”, enter analyst name and start date.

5.3.2 Obtain the specific product folder, which contains the Finished Product Specifications and Test Methods.

5.3.3 Enter the following sample information into the blank Product Test Record Form:

Product Name

Specifications Reference Number

Date

Batch / Lot Number

Product Type (e.g. Blend, Bulk and Finished Goods)

Test to be performed

Reference

Test Frequency

Specification of the test.

Note: The Laboratory Manager or designee should be consulted to clarify if full testing is required for this lot or whether the lot is part of the reduced testing program.

5.3.3.1 A Product Test Record Sheet must be generated upon testing a blend sample.

5.3.4 Carry out the test by the test method listed in the Finished Product Specifications and Test Methods, document the testing in the Laboratory workbook as per standard procedure. Complete, sign and date all documentation as per Good Documentation Practices. On completion the laboratory analyst should perform the followings:

5.3.4.1 Open the product specific files and enter the sample lot number and the results into the required worksheets. The trend graphs should be updated with the new results entry.

5.3.4.2 Check the results entered in the corresponding trend graphs are within both the Upper Control Limit and Lower Control Limit.  If not, proceed as per section 5.3.8.

Note: There should be a few charts ready for use for individual and average test results; e.g. Active Assay Chart, Dissolution Chart and Moisture Chart.

5.3.5 Complete the Product Test Record form by entering the results, the Laboratory Workbook reference and test completion date in the corresponding section in the Product Test Record form, sign and date the entries.

5.3.6 Ensure the test results conform to the Finished Product Specifications, if not, proceed as per section 5.3.8.

5.3.7 The Laboratory Analyst should report the results with the same number of decimal places as the specifications (unless specified in the reporting criteria from the method).

5.3.8 The Laboratory Analyst must report any result that is out of specification, out of trend or any deviations from the testing to the Laboratory Manager or designee.

5.3.8.1 If the test result is out of either Upper Control Limit or Lower Control Limit, but within the Finished Product specifications, the Laboratory Analyst must note the out-of-trend result in the workbook.

5.3.8.2 If the test result is out of the Finished Product specifications, the Laboratory Analyst must raise and carry out an laboratory out of specification investigation for questionable result in accordance with appropriate procedure.

5.3.8.3 The Laboratory Manager or designee must notify the site management of any confirmed out of specification results.  Deviation and/or change requests are initiated when required.

5.3.9 Upon completion of all tests (both testing and reporting) in each stage of process, the Finished Product Specifications and Test Methods folder, the filled Product Test Record Form (Template – 005, 145 and 150), Laboratory Workbook with all attached print out proofs (i.e. HPLC integration and chromatograph reports, TLC photographs, spectrophotometer print outs, weighing print outs etc) and a retention sample must be submitted to the Laboratory Manager, Team leader or designee for review. No retention samples need to be prepared for liquid and paste products as packed product is used as retention sample for these products.

5.3.10 In the Finished products database:  enter finish date, workbook number, laboratory investigation and/or deviation numbers if applicable.

5.3.11 Any left over samples should be stored until sample is approved and released from the laboratory, before being disposed of as per standard procedure Disposal of Laboratory Hazardous Wastes.

5.4    Reviewing, Approval and Releasing

5.4.1 The Laboratory Manager or designee must review the results in the filled Product Test Record Form, the Laboratory Workbook and machine print outs against the Finished Product Specifications and Test Methods folder and check for the results entered in the excel worksheets and product database, for accuracy and completeness and to ensure all documents are signed and dated.

5.4.1.1 The Laboratory Manager or designee must check the test results against the specifications and trend charts to ensure that all results are within the specifications and /or control limits. When required must raise laboratory investigations and/or deviations as per section 5.3.8.

5.4.2    The Laboratory Manager or designee should approve the results as following:

5.4.2.1 Sign and date on all documentation reviewed.

5.4.2.2 Complete the Laboratory Documentation TEM-145 Finished Product Specification and Test Report and submit to laboratory supervisor for review of the test results.

5.4.3    The Laboratory Manager or designee should release the sample if the results are within the Finished Product specifications. If a sample results is out of specification it is required to reject according to standard reject procedure.

5.4.4    The Laboratory Manager or designee should hand the retention sample to the Laboratory Attendant or designee for retention storage.

5.5    Document Filing

5.5.1 The Laboratory Workbook should be filed in the filing compactuses and product folder should be filed in the Products filing cabinet.

5.5.2 The completed Laboratory Documentation such as TEM-145 Finished Product Specification and Test Report should be given to the Laboratory Administrator or designee for generation of a Certificate of Analysis (COA).  Once the COA has been approved, the completed Product Test Record Form, Laboratory Document Check List and COA should then go to Quality Assurance for review.

5.6    Generation of COA

5.6.1 Upon receipt of the completed TEM-145 Finished Product Specification and Test Report , the Laboratory Administrator or designee should generate a COA from the appropriate template  The COA should contain the following information:

Product Name

Lot Number

Date Manufactured

Date of Analysis

Reference to the Corresponding Material Specification

Test / Method / Specification / Result

Statement of Quality

Signature of the Authority.

5.6.2 The Laboratory Manager or designee should review and sign the COA.

5.6.3 When the Quality Assurance signature is not required the Laboratory Administrator or designee should scan the COA and store the electronic copy in the relevant product folder. The hardcopy of COA will be attached to the Product Test Record and send to QA.  QA to file the hardcopy with the batch documents.

5.6.4 When the Quality Assurance signature is required the printed COA will be attached to the Product Test Record and forwarded to Quality Assurance department.

5.6.5 Quality Assurance Department to sign the COA, scan it and store the electronic copy in the relevant product folder. The hardcopy of COA will be attached to the Product Test Record and filed with the batch documents.

5.7    Reassay Procedure

5.7.1 Manufactured Semi Finished Goods

5.7.1.1 A reassay might be required if the bulk product is not packed within the specified time period listed in the Bulk Holding Periods.

5.7.1.2 If a reassay is required the Quantity and shelf life of the product is to be reviewed by the Supply planner.  The product needs to have more than 2 years shelf life in the market and the value of the product should be higher than retest cost.

5.7.1.3 The Supply Planners will alert Laboratory Manager and Manufacturing Department if a reassay is required on a manufactured semi-finished good.

5.7.1.4 Manufacturing Department will take samples from each drum and create a composite sample.

5.7.1.5 The reassay sample will be tested according to the relevant Finished Product Specifications and Test Methods.  Additional stability indicating tests are carried out based on stability protocol for the product; e.g. degradation products.  Identity tests will not be carried out.  In addition, capsules will be tested for brittleness.

5.7.1.6 When testing is complete the Laboratory Manager or designee will extend the due date for the bulk batch and on the List of Bulk Holding Periods.

5.7.1.7 New COA will be generated according to section 5.6.