Test expiry date

Implementation of this procedure precludes the necessity of giving expiry dates for these substances. However, no studies are undertaken to test the stability of the substance in opened vials or ampoules nor the substances in solution. Users of reference substances should not store solutions of chemical reference substances or opened vials. 

Calibration of dissolution equipment. It is very important to ensure that the calibration of the dissolution equipment is kept up to date. The expiry date of the calibration status should be checked each time that dissolution testing is performed. 

A brief description of the IR products used for dissolution testing, including information on batch or lot number, expiry date, dimensions, strength, and weight... 

Laboratory controls (testing of intermediates and APIs, validation of analytical procedures, certificates of analysis, stability monitoring of APIs expiry dating, retention samples)... 

Yang W-H, Roy SB. Projection of tentative expiry date from one-point accelerated stability testing. Drug Dev Ind Pharm 1980 6(6) 591-604. 

Where the final item being shipped consists of a collection of units, the final pack may often comprise different items that each have different expiry dates and batch numbers. Records that are held within supporting computer applications should accurately reflect the lot number and expiry dates for all of the elements contained within each pack to facilitate traceability. Once the pack has been produced and entered into the system as an item in its own right, the expiry date shown in the system for the pack and on its external packaging should be the earliest component expiry date. This should be verified as a specific test case during OQ and PQ testing. 

Normally the first three commercial production batches should be included in the stability-monitoring programme to confirm the expiry date. However, where data from previous studies, including pilot batches, show that the product is expected to remain stable for at least two years, fewer than three batches can be used. The testing frequency depends on the characteristics of the herbal medicinal products and should be determined on a case-by-case basis. 

The multisource pharmaceutical product used in the bioequivalence studies for registration purposes should be identical to the projected commercial pharmaceutical product. Therefore, not only the composition and quality characteristics (including stability), but also the manufacturing methods (including equipment and procedures) should be the same as those to be used in the future routine production runs. Test products must be manufactured under GMP regulations. Batch-control results of the multisource product, and the lot numbers and expiry dates of both multisource and comparator products should be stated. 

A documented, on-going testing program should be established to monitor the stability characteristics of APIs, and the results should be used to confirm appropriate storage conditions and retest or expiry dates. The test procedures used in stability testing should be validated and should be indicative of stability. 

Neither of these three questions is directly and expressly regulated by the GLP Principles. While the general data on the test item itself will have to be known (or at least be estimated) before the study actually starts (see the requirement for the labelling with an expiry date), this question becomes less... 

The requirement to provide an expiry date not only in the test item documentation, i.e. on the analysis sheet, but to print it plainly on the label of the test item container is a very important issue. It has to be seen in the line of all the other requirements for test item characterisation, namely to provide assurance that in the study the correct, unchanged, i.e. unadulterated and undegraded, test item has been applied to the test system in its original state. Since study personnel may not be able to consult the analysis sheet before each use of the test item, the requirement to print this information on the label of the test item container should thus ensure that in no instance a test item will be applied to a test system, the stability, purity and decomposition status of which could be in doubt. 

There are two points which need to be addressed in this context. In the first instance, the requirement for an expiry date is not confined to the labelling of test and reference items, but is also applicable to any chemicals, reagents and solutions used in a GLP compliant test facility. This issue has already be touched upon briefly in section 6 (see page 181). While there is no... 

Records including test item and reference item characterization, date of receipt, expiry date, quantities received and used in studies should be maintained. 

The expiry date becomes a simple problem when the producer is sure to sell all his material in a period where the stability test can still be performed. An answer could be to reduce the size of the batch so that the market can absorb it within two or three years. This would be a situation similar to pharmaceutical production where frequency of production and size of batch are market driven. Unfortunately, CRM production is a costly business. In particular for many matrix CRMs the end-user population is limited. Having larger batches of CRMs allows a decrease in the cost per unit. Decreasing the batch size will increase the cost of the CRM for the end user. Such cost would become unacceptable for measurements performed in highly specialised fields with limited numbers of laboratories (e.g. toxins, dioxins etc). 

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