Sample preparation in pharma quality control

Chromatography Forum: LC Archives: Sample preparation in pharma quality control
Top of pagePrevious messageNext messageBottom of pageLink to this message  By Sample on Thursday, March 18, 2004 - 07:03 am:

What is the best procedure to extract API from tablet matrices:
a) to add up to a defined volume (volumetric flask) or
b) to add a defined extraction volume to the sample (pipette),
if the tablet is based on mannitol and contains about 5% (m/m) insoluble excipients?


Top of pagePrevious messageNext messageBottom of pageLink to this message  By DR on Friday, March 19, 2004 - 05:40 am:

My personal preference is to add by pipet (for example: pipet 25mL into a 50mL vol. flask, add n accurately weightd tablets...)


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Sample on Tuesday, March 23, 2004 - 05:06 am:

In my lab itīs also common to add a defined volume. But do you know, why?


Top of pagePrevious messageNext messageBottom of pageLink to this message  By DR on Tuesday, March 23, 2004 - 12:02 pm:

It's probably because the insoluble excipients would throw off the volume your API was dissolved in if you were to QS flasks with extraction solvent. It would be by a trivial amount in most cases, but if you have a horse sized pill with a low concentration API in a small vessel, it could pose a significant systematic abberation from the accurate result desired.

It's also a bit easier in terms of sample prep - drop tablet(s), add fixed volume, shake and/or sonicate, filter, shoot.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By A.Mouse on Saturday, March 27, 2004 - 10:33 pm:

You are ultimately reporting all your data with respect to a defined volume of sample. The most accurate way to make up a sample with a controlled volume is to use a volumetric flask. It is simply fundamental good practice in a chemistry lab.

While it is not very likely to be important in your environment, assume for a second that you have two tablet making machines. One makes pills with a volume of 1 mL, the other one with a volume of 0.2 mL. Both are making tablets with a content of active ingredient of 20 mg.
If I use the approach advocated here and I dissolve the pills in a volumetric flask that will be filled to 50 mL, I get the same result for the analysis of both pills. If I use your approach - adding 50 mL of solvent to each pill, my analytical results will be different, and I have the QC department scratch their heads why the 1 mL pills don't pass specs.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Sample on Monday, April 5, 2004 - 08:28 am:

I agree with you at least partly. But what if your pills are made of mainly insoluble excipients - as DR wrote, these excipients would throw off some volume - like placing stones in your flask....?


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