LAB-005 Retest Dating of Raw Materials

1. Expired Stock Report

1.1. The Laboratory Manager or delegate at the beginning of each month will run the “Finished Goods Batches with Impending Expiry” report, which includes both raw materials and finished goods.  The report includes Product/Raw Material code, Description, BPN/Lab. number, Location number, quantity, Value of Item and Expiry date. This procedure is outlined below.

1.2.  RAW MATERIALS –include Active Ingredients, excipients and intermediates.  Retesting is performed to extend the shelf life.  These have a maximum initial retest period of X years providing supporting stability data is available.

1.3. FINISHED GOODS – This includes both local, imported and contract finished goods.  They are rejected if past minimum Expiry Date and not sold.

2. Raw Materials Approaching their Retest Date

2.1. All chemical Raw Materials used in products bear a date (Retest Date) after which they may not be used in a batch without further testing.  Once the Raw Material has reached its retest date, it may be retested and a new retest period assigned.

2.2. The retest date for a raw material and testing regime required for retesting is determined from the relevant Raw Material Specification – Test Report document (e.g. RM-XXX-YY.A). See SOP QMS-030 & TEM-005.

2.3. A retest date is determined by:

a)    Assigned by vendor (e.g. C of A)
b)    Based on in-house or Vendor stability data
c)    Assigned in accordance with the tightest international product registration requirements
d)    If a), b), and c) do not apply, 3 years then testing every three months or longer based on available data on a case by case basis.

2.4. At the beginning of each month, it is the Laboratory staff’s responsibility to check via Form-240 all Raw Materials that are due to expire in the following month.  After consultation with the Laboratory Manager, a decision based on Section 3 and 4 is made as to which Raw Material is to be extended and which is to be rejected.

3. Non Chemical Considerations for Raw Material Retesting

3.2. Is the Raw Material going to be used up in that month by Production?If yes, no retesting is required.

3.3. Is the amount and/or cost of Raw Material left worth testing? If it is, retesting is required. If it is not, a decision is made by the Laboratory Manager to reject the Raw Material item.

3.4. Is the Raw Material the only batch listed in the form?

a. If it is, retesting is required.

b. If it is not, a decision is made by the Laboratory Manager to reject the Raw Material item.  It may be that there are several batches of raw material in the system, is it likely that all batches are going to be used before expiry?  It could be appropriate to keep only one batch and reject the rest of the batches if for some reason production use has decreased.

3.5. Is the Raw Material still required by Production?

If the raw material is not in the bill of materials for any product (See SOP QMS-030 confirm with the appropriate planner/buyer if the material is required, and arrange a Deviation Report to be raised to write off the raw material from the inventory list.

3.6. Is the Raw Material a Trial?

ALWAYS retest as this gives real time for stability shelf life and for use as a secondary standard.

3.7. Is the Raw Material more than five years old? See Section 9.

4. Chemical Considerations in Raw Material Retesting

4.1. Available stability data.

4.2. Retest data/results comparison with previous analysis.

4.3. Available retest data from previous batches.

4.4. Stability indicating methodology.

4.5. Storage conditions of the Raw Material.

5. Retesting of Raw Material

5.1. If the Raw Material is to be retested it is sampled and retesting is carried out to the requirements in the Raw Material Specifications and Test Report to extend shelf life.  The approximate amount needed for re-testing can be calculated from the Raw Material Specification and Test Report (TEM-005).

5.1.1. Fill out ‘Expired Raw Material Form’ Form-335 with all the required information.

5.1.2. Send the Form-335 and Form-010 to Warehouse sampling personnel for re-sampling (see SOP WAR-010). The re-sampled Raw Material and Form-335 are returned to the Laboratory for testing.

5.1.3. The Laboratory staff tests the re-sampled Raw Material according to the Raw Material Specification and Test Report (TEM-005) for that particular material number.  Testing is carried out as per SOP LAB-070.

5.2. If the Raw Material Passes Retesting

5.2.1. If the Raw Material passes the testing, the Form-335 is placed in the “Raw Materials for Passing” tray for release by the Laboratory Manager.

5.2.2. The Laboratory Manager checks the results in Form-335 against the TEM-005 and if the raw material conforms, a PASS status is assigned to the Raw Material.

5.2.3. A new retest date is assigned and is calculated from the extension of shelf life period added to the date of completion of analysis.

5.2.4. The Laboratory Manager then signs Form-335.

5.2.5. The Laboratory Manager or delegate will inform Production planner about the current status of the raw material batch and verifies the retest details have been updated.

5.2.6. The completed Form-335 is filed in the Retested Expired Raw Material folder in alphabetical order kept in the Laboratory office.

5.3. If the Raw Material Fails Retesting

5.3.1. If the material fails retesting, the Laboratory staff alerts the Laboratory Manager of the failure and follows the procedure outlined in SOP LAB-065.

5.3.2. The Quality Assurance Manager or the Laboratory Manager must be advised immediately of any test during the re-examination that fails to comply with the Raw Material Specification.  This may necessitate a reduction in the shelf life for the material and/or placing finished good batches made with it under Quarantine until a firm decision is made.

5.3.3. If the Raw Material subsequently fails testing it is to be rejected and all batches in which it was used will be referred to the Quality Assurance Manager for evaluation.

5.3.4. If the Raw Material is to be rejected due to reasons described in section 3 and 4 or the Raw Material fails retesting, the raw material is given a FAIL status on Form-335.

5.3.5. The Laboratory manager raises a Deviation Report (see SOP QMS-035) which is noted on Form-335 and also informs the planner/buyer to ensure that potential disruptions to production scheduling are minimised.

6. Use of Raw Material Before Retesting

6.1. If a Raw Material has to be used after its expiry date, but before a new expiry date has been assigned, a Deviation Report must be raised (see SOP QMS-035) outlining justification of why the raw material may be used.  Consideration should be given to Section 7.  Approval must be sought from the Laboratory Manager before the Raw Material is used in production.

6.2. The finished good batch must also be placed on the Stability Data program.

7. Documentation of Retest Period

The rationale used to determine the retest period shall be documented.  The approval shall:

7.1. Avoid “1 batch testing”.

7.2. To assure continued stability and avoid one batch testing, a stability profile of the active can be built up using extended stability products.  Where stability limited stability data is available, further supporting data can be obtained such as analysis of samples from stock of batches of similar age and an evaluation comparing impurity levels and profiles with original results.

7.3.  Evaluate the effect of ageing on the physical parameters of the material.

7.4. Consider final usage form of the product.

7.5. Consider the conditions in which the active has been stored.

7.6. Consider the Regulatory implications.

8. Changes to Initial Retest Periods

8.1. Permanent extensions to assigned initial retest periods may be made where satisfactory evidence is available to support the changes.  For an active such evidence is typically data from stability programmes, but may also include real time testing of material in stock.  Any change must be made via the change management system in order that it is subject to regulatory compliance and to ensure that all relevant documents and systems are updated.

9. Use of Raw Materials Greater than 5 Years of Age

9.1. The approval of a raw material beyond 5 years of age shall be considered and evaluated on an individual basis.  Beyond 5 years, due to the age of the material, the rationale shall be documented and a DR raised against the batch being manufactured with the Raw Material.  Approval shall be gained from the Quality Assurance Manager before the Raw Material is used in production.  Considerations given in Section 7 shall be applied.

9.2. When using raw materials greater than 5 years in age, consideration shall be given to:

a. Formulating under experimental programme to monitor the affect on manufacturability/material behaviour;

b. Placing formulated product on stability.

10. Summary of Changes