It is ALL relative. According to various regulations cleaning validation refers to the API (because it has a known physiological effect as determined by clinical studies), cleaning agents (thus sampling after a WIFI rinse), or Micro.. You could have a placebo peak, solvent peak, injection peak (you have your work cut out)
WRONG! Acceptance criteria are HARD limits since they are based on the toxicity of the molecule (whether API, cleaning agents...). Thus, the swab limit, maximum safe concentration (MSC not MACO), HBEL (health based evaluation limits) are derived from the toxicity (even for generic drug products).
Hi Dr. Mahmoud,
In general, no extra peak should be detected in the CV sample. If any, it should be less than the quantitation limit (QL) established at your end.
Some pharmaceuticals are using the limit < 30% w.r.t MACO limit, as it recommended by ICH guidelines for similar cases, e.g., elemental impurities.
If you want to identify or characterize the impurity, you could use the LC-MS for the mass value confirmation and and LC-MS/MS fragmentation patterns, so that you could assess / predict the chemical structure almost 90%. If you would like to know the complete structure info, you could collect the extra peak fraction and concentrate it, and then perform the NMR (1-H & 13-C).
Thanks!
Dr. Narasimha S.
▪️connect the HPLC directly to a mass spectrometer (LC-MS).or
▪️take your HPLC method with a known amount of active component spike it and perform the HPLC analysis
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