Accelerated Degradation Experiment
Conditions
Procedure A: |
30 days exposure at 50 °C and 100% relative humidity. |
Procedure B: |
30 days exposure at 50 °C and 100% relative humidity followed by 5 days at 70 °C and 100% relative humidity. |
Appearance of the material
The material, originally in the form of a pale grey to brown-yellowish powder changes after procedures A and B into a dark brown paste.
Gain of moisture
After procedures A and B: |
30 - 45% |
Chromatographic test
Adsorbent: Silica gel 60 F-254
Solution applied to the plate: Chloroform layer after extraction of the material with ammonia.
Solvent system:
toluene ............................35 volumes
benzene ...........................35 volumes
ethyl acetate ....................20 volumes
diethylamine ...................10 volumes
methanol ...........................2 volumes
Development condition: The solvent is allowed to migrate until the front reaches a line 15 cm from the starting line.
Detection: The plate is examined under ultraviolet light at a wavelength of maximum output at about 254 nm and then at 365 nm. After spraying with a solution of potassium iodobismuthate the plate is examined at 365 nm.
Results: The reference solution of ipecacuanha shows numerous spots of different intensities depending on the detection method. The spots obtained from the solutions of each of the samples subjected to procedures A and B correspond in number and position to the reference solution, but the intensities are considerably and irregularly modified.
Gas-liquid chromatography
The chromatograms of solutions of samples subjected to procedures A and B are modified significantly, the size of the main peaks, corresponding to emetine and cephaeline, decrease, whereas the unidentified secondary peaks increase considerably in intensity.
Conclusion
Ipecacuanha is subject to decomposition under accelerated degradation conditions.
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