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In soluble product - Residual solvents
Posted: Mon May 07, 2007 8:56 am
by bioram
Hai,
There is a problem for analysis of residual solvents of my drug substance Buclizine .
This substance is not soluble in any solvent. It is sparingly soluble in propaediol, ethanol.
To analyze residual solvents for this product how can I perform sample preparation .
It was not soluble in any solvents like DMF, DMSO, NMP and other organic solvents.
HS residual solvents
Posted: Mon May 07, 2007 12:52 pm
by chromatographer1
At what temperature does the product melt?
best wishes,
Rod
Posted: Mon May 07, 2007 1:00 pm
by chromatographer1
Is
Buclizine , or 1-(p-tert-Butylbenzyl)-4-(p-phenylbenzyl)piperazine dihydrochloride
soluble in water?
soluble in water at 80°C ?
Do you know at what levels it is soluble at these conditions?
best wishes,
Rod
Posted: Mon May 07, 2007 1:03 pm
by chromatographer1
another suggestion is to try to dissolve Buclizine in water: DMAc, 1:1, and heat it to 80°C 10mg per 100 µL or 500 µL
If you have to use a concentration of less than 0.1mg/mL you could always use SPME headspace.
best wishes,
Rodney George
Senior Research and Development Scientist
Gas Separations Research
Supelco
595 North Harrison Road
Bellefonte, PA 16823
814-359-5737 voice
814-359-5459 fax
rodney.george@sial.com
Posted: Tue May 08, 2007 1:58 pm
by Charles A. Burger
Is the analysis by headspace. If so, waybe benzyl alcohol. I had a similar situation with a compound that was slightly soluble in ethanol. I went with benzyl alcohol and it went into solution after heating to 80°C.
Chuck
Posted: Wed May 09, 2007 5:16 am
by bioram
It is not soluble in water at any temperature
thank you for your suggestion ROD
Posted: Wed May 09, 2007 12:27 pm
by chromatographer1
Let me know the melting temperature.
If it is reasonable <120°C you could do headspace analysis just by melting a 1-10mg sample in a vial.
best wishes,
Rodney George
Senior Research and Development Scientist
Gas Separations Research
Supelco
595 North Harrison Road
Bellefonte, PA 16823
814-359-5737 voice
814-359-5459 fax
rodney.george@sial.com
Posted: Mon May 21, 2007 9:45 am
by Peter Apps
With the appropriate precautions and very long equilibrium times you might be able to do the analysis by equilibrium headspace over a powdered sample.
Peter
Posted: Mon May 21, 2007 11:00 am
by bioram
Thank you peter for your valuable suggestion
I will come back after conducting the experiments.
rama krishna