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how to improve low level spiked recovery-urgent!

Discussions about HPLC, CE, TLC, SFC, and other "liquid phase" separation techniques.

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I am validating a drug product impurity method. The spiked recovery was performed by spiking a known impurity at LOQ level (1%), specification limit (3%) and 5% to placebo which contains water, API and mannitol. API was also spiked along with the known impurity to demonstrated recovery of unknown impurity. (for ex: spiked both know imp and API at LOQ level to 40ug/ml mannitol in water). The recovery criteria is 85-115% but the spiked recovery for known impurity failed at LOQ level while API passed.
This is a lyophilized drug and suppose to be reconstituted with water before administered.

Why is the known impurity recovery low at low level? I can only think of two reasons: 1 impurity was binding with mannitol, 2: impurity was not completely dissolved. Either way I think I should look into sample preparation? maybe sonicatethe sample (the sample was not sonicated at the time of prep)?

Pleas advise on how do I improve the recovery? and what could be the reason.

Thanks.
Maybe it’s a LOQ issue? Try and double the spiked amount to see if it doesn’t improve the situation.
Best Regards
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Dancho Dikov
2 posts Page 1 of 1

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