how to obtain the degraded product

[vshyam81]

respected forum...,

myself a master of pharmacy student from india would like to clear a query about separating my degradation product for HPLC,NMR and LC-MS.

Readers, i do perform my dissertation work in development of a stability indicating method using chromatographic methods for anticancer drugs.

as, my stability studies have come to an end and i would like to isolate my degradant by completly degrading my drug.for tht i used hydrogen peroxide and applied high conditions for degradation,but the problem arises tht after degradation am unable to separate my degradant from hydrogen peroxide,i did employ heating to dryness and vaccum dring too in both cases the result was tht the hydrogen peroxide just made foam and left but nothing remained in the round bottom flask.

as my drug is acetonitrile and methanol soluble i tried using the solution for extraction then as the result was similar to as i mentioned above,i changed my procedure as taking the drug 50 millgram and directly adding hydrogen peroxide and doing degradation. the results obtained are as mentioned above.
respected readers i would like know or would request u r help to solve this problem...

thanking you,

vivin

[yogesh#14]

Hi ,

After redaing your query , i would like to suggest you that you boil off your solution after adding peroxide. I guess you should try high concentration on preparative HPLC. Since you want to isolate the impurity you will have to SCALE UP your HPLC method.

or else you can load a high volume concentration and collect the eluent a nd evaporate to get the desired impurity,

hope this will help u...

Yogesh

[Matt Savage]

I not sure I entirely followed what you were wanting (I'm a simple polymer chemist!) but is there any reason you can't add a tiny ammount of Manganese Oxide to the degraded product and convert the peroxide to water and oxygen?

[DR]

Patience and semi prep. HPLC may be required unless you get to where you understand the reaction pathways to get to your main degradation products, if you have that and a stability indicating method, you can optimize stress induced production from the drug or a synthesis route (know any good synthetic organic chemists?).

[Bruce Hamilton]

Have you got a project manager or supervisor you can discuss the problem with?. Once you've degraded the compound using standard conditions, you want to be really nice to it so you don't form other degradation products that you will not be able to explain. You should not be trying to heat the sample further to drive off the H2O2, for reasons that you're just discovered...

I assume that you've analysed a small fraction of the degraded sample and measured the decrease in your anti-cancer drug before you tried to recover the bulk?. If that decrease is large, and the degradation peaks are well away from the main compound, then you may be able to use simple column/flash/spe systems to separate your degradation products. If not, then preparative HPLC may be your best choice.

You really should be talking to your project supervisor. When in a hole, don't keep digging...

Bruce Hamilton