During the development process of an oxycodone tablet, a New Jersey based pharmaceutical company became concerned that their Active Pharmaceutical Ingredient (API) was possibly degrading. Since the FDA requires reporting of any degradation product exceeding the threshold of 0.05% and identification of all impurities greater than .1% for a daily dose drug product that is less than two grams per day; the client requested Avomeen to identify and quantify any product degradation that may be present.
Avomeen’s chemists used High-Performance Liquid Chromatography (HPLC) to compare the client’s tablet against a standard Oxycodone sample. The HPLC chromatograph of the tablet revealed four minor peaks in addition to the expected Oxycodone peak. The quantification of these impurities was greater than 0.1% of the total composition, requiring identification of the impurities.
In order to identify the impurities, the sample was run using Liquid Chromatography-Mass Spectrometry (LC-MS). LC-MS revealed one of the four unknown peaks to be Toluene, a residual solvent which was used in the manufacturing process of the tablet. The second and third peaks were classified as oxidation products of the oxycodone, while the fourth peak was determined to be a substituted oxycodone.
Our chemists synthesized several potential oxidation products of oxycodone to use as reference standards in order to identify the degradant oxidation products. HPLC was then performed on the synthesized reference standards and the retention times were compared to those of the impurities in question in order to determine a match. By repeating this process with each synthesized oxidation product of oxycodone, the chemists found a positive match thereby identifying the degradation product.
The identified oxidation product was a known compound which was harmless to consumers. Since this impurity was determined to be in such a small quantity there was no concern that it caused any issue towards the safety or effectiveness of the pharmaceutical product.
Avomeen’s chemists successfully determined that the pharmaceutical manufacturer’s API did degrade, but that the degradation products present were of no threat to the drug’s safety and efficacy. This allowed our client to continue their production process without delay and produce their product with full confidence in its safety.
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