Meet ICH2003 Q1A(R2), CP2010
(1) Accelerated test: 40℃±2℃ / 75%RH±5%RH
(2) Intermediate conditions: 30℃±2℃ / 65%RH±5%RH
(3) Long-term test: 25℃±2℃ / 60%RH±5%RH or 30℃±2℃ / 65%RH±5%RH
1. High temperature test
The test sample is placed in a suitable sealed clean container at 60℃ for 10 days. Samples are taken on the 5th and 10th days and tested according to the key stability inspection items. If the test sample has obvious changes (such as a 5% decrease in content), the same method is used to test at 40℃. If there is no obvious change at 60℃, the 40℃ test is no longer performed.
2. High humidity test:
The test sample is placed in a constant humidity sealed container and placed at 25℃ under the condition of relative humidity of 90%±5% for 10 days. Samples are taken on the 5th and 10th days and tested according to the requirements of the key stability inspection items. At the same time, the weight of the test sample before and after the test is accurately weighed to inspect the moisture absorption and deliquescence performance of the test sample. If the moisture absorption weight gain is more than 5%, the test is carried out in the same way under the condition of relative humidity of 75%±5%; if the moisture absorption weight gain is less than 5% and other inspection items meet the requirements, this test is no longer carried out.
3. Strong light irradiation test:
The test sample is placed in a light box equipped with fluorescent lamps or other suitable lighting devices and placed under the condition of illumination of 4500lx±500lx for 10 days. Samples are taken on the 5th and 10th days and tested according to the key stability inspection items. Special attention should be paid to the changes in the appearance of the test sample. In addition, according to the nature of the drug, experiments can be designed when necessary to explore the effects of pH, oxygen and other conditions on drug stability, and to study the analytical methods of decomposition products.
4. Accelerated test:
This test is conducted under extraordinary conditions. Its purpose is to explore the stability of the drug by accelerating the chemical or physical changes of the drug, and to provide necessary information for drug review, packaging, transportation and storage. It is required to provide 3 batches of test products in commercial packaging, which are placed for 6 months at a temperature of 40℃±2℃ and a relative humidity of 75%±5%. The equipment used should be able to control the temperature ±2℃, the relative humidity ±5%, and be able to detect the actual temperature and humidity. During the test period, samples are taken once at the end of the first month, second month, third month, and sixth month, and tested according to the key stability items.
5. Long-term test:
5.1 Long-term test is conducted under conditions close to the actual storage conditions of the drug, and its purpose is to provide data for formulating the shelf life of the drug. The test sample requires 3 batches, commercially available packaging, and is placed at a temperature of 25℃±2℃ and a relative humidity of 60%±10% for 12 months. Samples are taken every 3 months and tested according to the key stability inspection items at 0 months, 3 months, 6 months, 9 months, and 12 months. After 12 months, further inspections are required at 18 months, 24 months, and 36 months, and samples are taken for testing. The results are compared with the data of 0 month to determine the shelf life of the drug.
5.2 For drugs that are particularly sensitive to temperature, long-term tests can be placed at 6℃±2℃ for 12 months and tested according to the above time requirements. After 12 months, further inspections are required according to regulations to formulate the shelf life under low temperature storage conditions. The packaging used for accelerated tests and long-term tests of raw materials should use simulated small barrels, but the materials and seals used should be consistent with large barrels.
