QCS-014 - Quality Operations Procedures for Pharmaceutical, API, and Biotechnology - page 72

SOP No. QCS-014.00 Effective date: mm/dd/yyyy
Approved by:
14.4.4.1 long-term testing
Long-term tests must be carried out on representative batches using the type of packages intended for
marketing. A 12-month long-term stability data should be provided at the time of submission. In this
case, the storage is carried out at 30°C ± 2°C/60% RH for solid phase and 30°C ± 2°C for liquid
phase. This should be done for all types of drug products and the study should cover not less than 12
months duration at the time of submission for registration, provided that the manufacturer has to give
a written assurance that long-term testing will continue to cover the expected shelf life completely.
In this type of study, the observations and testing are done first at zero time, every 3 months during
the first year, every 6 months during the second year, and then every year till the end of the shelf life.
14.4.4.2 short-term or accelerated stability testing
a. A 6-month accelerated stability data should be provided at the time of submission for registra-
tion which should be carried out at the following storage conditions: 40°C ± 2°C/75 + 5% RH
for solid sample and 40°C ± 2°C for liquid sample and 3 months date for samples stored at
50°C ± 2°C.
b. For products to be stored for long term under refrigerated condition, the accelerated testing
should be conducted at
25°C ± 2°C
20°C ± 2°C
c. In these accelerated stability studies, the storage under high humidity applies particularly
to solid dosage forms which are not packed in containers designed to provide a permanent
barrier to water loss. For such formulations, the relative humidity should be lowered by
10-20%.
d. For some dosage forms, especially liquid and semisolid dosage forms, the study design
may also need to consider low-temperature freezer (−10°C to −20°C) and refrigerator (2°C
to 8°C), but usually, accelerated studies are less suitable for semisolids and heterogeneous
formulations, for example, emulsions.
e. Other storage conditions in stability studies are allowable if justified. The heat-sensitive
drug products should be stored under an alternative lower-temperature condition, if justi-
fied by the manufacturer, which will eventually become the designated long-term storage
temperature. Studies at low temperature that affects and changes the finished product's
properties should be avoided.
f. For products such as solutions, suspensions, and so on contained in packs designed to pro-
vide a permanent barrier to water loss, specific storage, under condition of high relative
humidity, is not necessary.
14.4.4.3 for (routine) ongoing stability studies
14.4.4.3.1 On Retained Batches Obtained from Current Production
a. Zero-time result will be taken from the QC department “release result.”
b. Every year, for some products, one batch will be selected from the sample reference room
in QC, which is near to expiry for analysis by the stability staff.
14.4.4.3.2 Stability Data for Supplemental Changes
Stability data submitted in support of supplemental changes for an existing drug product may be
generated with samples at the accelerated testing conditions and long-term testing conditions.