Accelerated Degradation Experiment
Conditions
Procedure A1: |
10 days exposure at 50 °C and 100% relative humidity. |
Procedure A2: |
20 days exposure at 50 °C and 100% relative humidity. |
Procedure A3: |
30 days exposure at 50 °C and 100% relative humidity. |
Procedure B1: |
30 days exposure at 50 °C and 100% relative humidity followed by 4 days at 70 °C and 100% relative humidity |
Procedure B2: |
30 days exposure at 50 °C and 100% relative humidity followed by 7 days at 70 °C and 100% relative humidity. |
Appearance of the substance
The substance, originally in the form of a white, crystalline powder, changes after procedures A and B into a colourless liquid.
Gain of moisture
After procedure A1: |
49% |
After procedure A2: |
59% |
After procedure A3: |
62% |
After procedure B1: |
62% |
After procedure B2: |
44% |
Chromatographic test
Adsorbent: Silica gel F-254
Solution applied to the plate: Substance dissolved in methanol.
Solvent system:
diethylamine ................ 1 volume
xylene .......................... 10 volumes
methanol ....................... 3 volumes
ethylmethylketone ......... 10 volumes
Development conditions: The solvent is allowed to migrate until the front reaches a line 10 cm from the starting line.
Detection: The plate is examined under ultraviolet light at a wavelength of maximum output at about 254 nm, then left in a chromatographic chamber containing some iodine crystals until spots appear.
Results: The spots obtained from the solutions of each of the samples subjected to procedures A and B, and the spots obtained from the reference solution of pethidine hydrochloride display the same spots are revealed.
Non-aqueous titration of the free base
No degradation is observed
Conclusion
No decomposition is detected by thin-layer chromatography and non-aqueous
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