Normally Using placebo spiked with drug powder as samples only works for immediate release forms since they disinteregate anyways. But what is to be done for XR tablets ? Would spiking method work again ?
What if all the drug is released within the first hour but the method was supposed to check till 10 hr?
Pls dont refer USP , i can't find a straight answer there.
Yes, the accuracy is always done by the spiking method. For XR, extend the spiking limit to lower concentrations.
Dear Sagar, I'm affraid I'm not sure I got your question properly. Are you willing (a) to validate the analytical method intended to quantify the dissolution samples, including the sample prep steps or (b) qualifying the dissolution apparatus.
In case is the former one, you have mainly 3 issues to deal with: (a) analytical accuracy (hplc, UV spectr, etc); (b) sample removal/filtering from dissolution vessel and short term stability and (c) solutions "long term" stability.
Aspect (a) you can demonstrate with synthetic solutions (api+matrix) and spiking. For (b) you need to take into consideration the dissolved/suspended excipients and their impact on the filtration/filter adsorption and analytical interference on the API quantification.
Regarding (c) you will need to ensure the samples stability in the dissolution medium (api+excipients) over time (at least 10 hours, in your case).
The proper experimental design will depend on your equipment setup and the time/materials available to perform the task (consider using whole tablets, crushed tablets and direct uncompressed raw materials). Hope it helps, Luis
Thank you Mr Luis.
I seem to be confused that validation needed to consider product characteristic too and was confused over losing the extended release property of my XR tablets with simply spiking API with excipients while checking accuracy of analytical method.. Now i understand that Accuracy determination for method validation does not need to consider if tablets are immediate. delayed or extended release since validation is not for the formulation but for the analysis method (UV or HPLC) and dissolution apparatus only.
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