Stability testing protocol

Q1A(R2) Stability Testing of New Drug Substances and Products Stability testing protocols including temperature, humidity, and trial duration... 

An extension of an expiration dating period based on (1) data obtained under a new or revised stability testing protocol that has not been approved in the application or (2) full shelf life data on pilot scale batches using an approved protocol. 

Stress testing is used to help identify degradation pathways under the influence of accelerated heat, light, and RH conditions in the presence or absence of air or oxygen. Such stability testing protocols represent an important aspect of a pharmaceutical ingredient process validation program. 

In addition to the ICH, the Committee for Proprietary Medicinal Products, under the European Agency for the Evaluation of Medicinal Products (EMEA), issued, in 1997 and 1998, a number of stability-related guidances to be used for establishing stability testing protocols for drug products to be filed in European countries. The documents complement and supplement the ICH guidelines and are listed below ... 

To illustrate the application of the Q-Rule, let us assume that the stability of a product at 50°C is 32 days. The recommended storage temperature is 25°C and M = (50 - 25)/10 = 2.5. Let us set an intermediate value of Q = 3. Thus, Qn = (3)2.5 = 15.6. The predicted shelf life is 32 days x 15.6 = 500 days. This approach is more conservative when lower values of Q are used. Both Q-Rule and the bracket methods are rough approximations of stability. They can be effectively used to plan elevated temperature levels and the duration of testing in the accelerated stability testing protocol. 

Chapter 5 extends the discussion on stability testing protocols to retest periods and elaborates on the procedures used for continued testing of products. 

A commitment is needed to place three commercial production batches under the same stability testing protocols. 

Written stability-testing protocols are available for all relevant tests. They are dated and signed. 

Stability Stability protocols and data should be submitted, along with the commitment and protocols to continue stability testing post-approval. 

Specialized LIMS— This type of LIMS is based on the fact that certain laboratories have a range of well-defined processes (e.g., stability testing) that are performed according to a specific set of regulations and by using well-established tests. The tests are done according to industry-wide accepted protocols. Specialized LIMS are tailor-made for certain types of laboratories. Therefore the performance can be optimized for clearly defined work process. 

Re-qualification (RQ) is a combination of OQ and PQ. This can be written as a separate protocol or can be included as part of the PQ protocol. This protocol can be executed anytime to demonstrate that maintenance has been performed, or periodically to demonstrate that the system is within tolerances. The RQ protocol should be able to be executed as needed without getting new signatures. Suppose the power supply has been corrected. An RQ protocol could include the high voltage accuracy and stability tests along with system suitability for one of the methods run on the system. This would demonstrate that the system is performing appropriately after the maintenance, as the manufacturer and you intend. 

The pH, solubility, volatility, and stability of a substance in test vehicles can affect the performance of mutagenicity tests and therefore influence the design of test protocols. 

Q1B Stability Testing Photostability Testing of New Drug Substances and Products Basic testing protocol required to evaluate light sensitivity and stability of new drugs and products... 

The so-called storage stability test is a standard test that is used across many different fields—e.g., the pharmaceutical, cosmetic, and food industries. The test is popular because it yields precise information about the long-term shelf life of emulsions. In this test, emulsions are stored under conditions that are applicable to those encountered in the actual production/consumption situation. It should be noted that the presented test protocol is time consuming and requires sampling over an extended period of time. In the... 

The test procedures described above (see Basic Protocols 1 and 2) have recently been simplified by utilizing advanced techniques such as ultrasonic and infrared spectroscopy. The purchase of one of these advanced analytical instruments is recommended for emulsion manufacturers that frequently conduct emulsion stability tests and require automated analysis of a large number of samples. 

Figure D3.4.7 showstypical results obtained from a storage stability test (see Basic Protocol 1) of an oil-in-water emulsion that consists of a 20% (v/v) hexadecane-in-water emulsion stabilized by 2% (w/v) polyoxyethylene-20-sor-...

As in the storage stability test (see Basic Protocol 1), the preparation time is short. Less than 30 min are required to set up the samples for storage. The actual storage stability for creaming profile determination is usually conducted over a periods of up to 4 weeks. Tests that are accelerated by centrifugation may require less than 8 hr of preparation and completion. 

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