In soluble product - Residual solvents

[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.

[chromatographer1]

At what temperature does the product melt?

best wishes,

Rod

[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

[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

[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

[bioram]

It is not soluble in water at any temperature

thank you for your suggestion ROD

[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

[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

[bioram]

Thank you peter for your valuable suggestion

I will come back after conducting the experiments.

rama krishna