LAB-065 Laboratory Testing and Documentation of Finished Products

1. Location of Samples to be Tested

1.1.  Finished Goods test samples are collected by an authorised laboratory staff form the retention sample room after signing the Test and Retention Sample log book and distributed to the appropriate teams and placed in the designated team sample drawers.

1.2. Stability and Trial samples are stored in the appropriate Stability Rooms, or in the fridge.

2. Location of Documentation for Samples to be Tested

2.1.  ‘Finished Product Specification and Test Report” (TEM-160) awaiting result entry is kept in designated labelled work files.

2.2.  Stability Cards and Trial Cards are filed in the stability filing cabinet.  The Stability and Trial cards requiring testing for that month are placed in the designated stability and trial cards (Form-315) work files according to the teams.  The teams collect the cards and the samples for testing.

3. Control Methods

Technicians must refer to the authorised copies of SOPs, Control Methods and FG Specifications; do not make lists of “handy hints”.

3.1. Finished Goods Control Methods are located in the filing cabinets and filed alphabetically.  Any Control Methods found to contain an error is brought to the attention of the Laboratory manager.  Master Document Change Control Form (Form-365) is generated by the Laboratory Technician to correct the error.

3.2. Control Methods to be used for Finished Goods, Trial and Stability testing, is established by Technical Service, QA and Laboratory teams as a part of master documents.

3.3.  Finished Good testing: Control Method to be used is noted on the Finished Product Specification and Test Report.
Trial and Stability testing: Control Method is noted on the card or Protocol.

4. Pre-Testing

4.1.  Note any unusual sample characteristics of the Finished Goods, Trial or Stability samples.

4.2.  Determine the type and sequence of tests to be performed.

4.3.  For each test, utilise the appropriate personal protective equipment.

4.4.  Set up the test equipment and ensure that it is within calibration.  If not, calibrate the equipment prior to use (see SOP LAB-010).

Do not use an instrument that is out of calibration to perform a test.

4.5.  Alert the Laboratory manager immediately if an instrument is failing its calibration.  The authorised laboratory technician arranges the service/repair of the equipment.  See SOP LAB-010.

5. Reagents Used in Testing

5.1.  Reagent solutions are made up according to the Finished Product Specification-Test Report and the corresponding Test methods.

5.2.  When a reagent solution requires standardisation, duplicate standardisations are performed according to the method.  Duplicate results should not differ by more than 2%.

5.3.  Reagent solutions used must be within the expiry date.

5.4.  See SOP LAB-035 for the preparation and storage of reagent solutions.

5.5.  See SOP LAB-040 for the disposal of Reagent waste.

6. Standards Used in Testing

6.1.  When a standard solution is prepared, the information and calculations relating to the standard must be recorded in the workbook.  See SOP LAB-025 on correct data entry into the workbook.

6.2.  See SOP LAB-035 for the preparation and storage of Standard solutions.

6.3.  Refer to SOP LAB-020 for the use and storage of Primary and Secondary Standards.

UNLABELLED CHEMICALS are a SAFETY HAZARD to others and ARE NOT PERMITTED.

7. Sample testing

7.1.  Perform the tests as specified in the Control Method:

a. ALWAYS duplicate testing for trials.

b. Single testing for Stability and Finished Goods unless specified.

7.1.1. Exceptions:

a. HPLC (chromatography) assays involving only one or two batches in the HPLC run (duplicates required).

b. Assays performed by manual titration (duplicates required).

7.2.  Establish the specification limits as follows:

a. Finished Product Specification and Test Report;

b. Stability/Expiry specifications for stability samples;

c. Trial specifications for trials.

7.3.  For duplicate assays:

Check that duplicates are within 2% of each other.  If not, see SOP LAB-055

7.4.  See SOP LAB-075 – for further information on stability testing.

7.5.  It is essential that work areas are clean and tidy at the end of the day.

7.6.   Equipment is to be left in a clean condition and ready for the next user.

7.7.   Tested Finished Goods are disposed in the appropriate security reject bin.

8. Within Specification Results

8.1.  Prior to reporting/entering results into FG Spec. and test report, check result(s) are within release specification limits.
For stability and trials only, check whether results are within 2% of previously obtained result(s).

8.2.  If result(s) are within specifications, record the result(s) obtained into the FG Spec. and Test Report, Trial or Stability Card, using the correct units. Analyst to Enter the results into finished Goods Trend Card (Form-260), sign and refer to the book page number of the work book.

8.3.  Stability or Trial Cards are signed and dated as correct by the analyst.

9. Out-of-specification (OOS) results

9.1.  Check that finished good result(s) are within specification limits.
Check that stability and trials results are within 2% of previously obtained result(s).
If any result is out-of-specification (OOS) for finished goods, stability and trials follow the procedure detailed in SOP LAB-055 using Form-305.

9.2.  Established that the laboratory determinate error has passed, retest the Finished Goods, Stability or Trial as per SOP LAB-055.

9.3.  Results not within specification follow SOP LAB-055. and record all details of the investigation on Form-305.

10. Documentation of Results

A workbook is a legal document.  All data is to be neat and legible.  Scribbles, liquid paper and pencil are not permitted.  Calculations are to be clearly shown.  Any mistakes in a workbook or a Results Recording Sheet when corrected are crossed out neatly, initialled and dated.  See SOP LAB-025.

10.1.  A numbered workbook including numbered pages is required to document/log all testing information, including out of specification investigation results.

10.2.  Information required in a workbook.
Finished Goods Name and Code Number, Batch Production Number, control method number/s, testing date and all raw testing data, e.g. weights, volume. The information regarding the standard used in the testing should be written down, for example, Batch Number or Lab. Batch Number, expiry date and assay.

10.3. All calculations and measurements are to be entered into the Analyst’s workbook.

10.4. Tests, e.g. Identity and Limit tests, can be directly entered onto the FG Specification and Test Report, Stability Card or Trial Card.  Terms such as “negative”, “positive”, “conforms” should be used to describe limit and identity tests.  All entries on FG Specification and Test Report, Trial Card or Stability Card are to be signed and dated.

10.5.  FTIR, UV/VIS, Particle Counters and Polarimeter etc results generated by a computer printout are attached to the FG Specification and Test Report.  The computer printout of the standardisation of solutions on the UV/VIS and Polarimeter are attached to the analyst’s workbook.

10.6.  A Finished Goods Trend card (Form-260) is assigned for each single finished Product. Laboratory staff has to fill up the test results accordingly form the workbooks and sign the card

10.7.  The FG Specification and Test Report is then filed in the appropriate work file.

11. QA Inspection Sheet

11.1.  After a finished product is tested according to corresponding “Finished Product Specification and Test Report” (TEM-160) the selective test results are to be entered into part B of “QA Inspection sheet” (Form-565). Authorised laboratory analyst should enter the results from the analyst work book and the completed Finished Product Test Report (TEM-160). The Inspection sheet has to be transferred to QA for final release of the Batch.

12. Microbiological Testing

Microbiological testing is required for various Finished goods.

Check the FG Specification and Test Report and if “MICRO STATUS” is required, send the required sample to in house or contract micro laboratories. Document the micro results on to the FG Specification and Test Report and on the trend card writing the contract laboratory reference no.

13. Completed FG Specification and Test Report

13.1. Completed FG Specification and Test Report are filed in the appropriate work file.

13.2.  Completed Stability and Trial Cards are filed in the completed file on the Stability/Trial work files.  Stability and Trial Cards are filed after reporting.

13.3.  Completed FG Specification and Test Report and the corresponding batch documents are matched.

14. Release of Finished Goods

14.1. The Authorised Person releases, or rejects the batch according to SOP QMS-075.

14.2.  The completed FG Specification and Test Report are filed in sequential order in appropriate filing cabinets.

15. Appendix 1 – Flowchart for Finished Goods

16. Summary of Changes