Advertisement

Doubt about the purity plot

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

5 posts Page 1 of 1
Hi, everyone!
I have a question about some purity plots obtained from an active ingredient sample subjected to forced degradation.

When running the degraded samples under various conditions, I encountered two unusual purity plots: the first related to degradation under alkaline condition:
https://ibb.co/6YxsddT

The second under acidic condition:
https://ibb.co/Hg6GWwb

Are these plots acceptable, or should something be done?

Thanks in advance.
They seem weird, but I'm not too much into it.

But a threshold of 90° doesn't look right. Check the window where the purity blank is measured. Probably there's a peak or strong absorbing background?

The second peak is obviously a shoulder, so expect a non-purity result, due to the contribution of the main peak.
Also check the PDA manual for the theory of Empower's purity algorithm, and also Waters Knowledge-DB articles WKB46540, WKB85832

https://support.waters.com/Special:Sear ... &type=wiki
There is absolutely no possible way anyone could answer this question without YOUR complete method details AND all of the Peak Purity settings, reference peaks and parameters used in your software and method. Many of the settings (and esp the 'default' values, many of which are just place holders for real values) are subjective, so the results obtained can easily be adjusted to show almost any desired result. For them to have any value, the method must be optimized, the purity settings carefully manually adjusted with clean reference peaks and the parameters optimized.

Also, a threshold of 90% seems very low to use.
Agreeing w/ ^^^, you have some work to do still and the more you don't tell us, the more we can't help you.
Thanks,
DR
Image
It is unnecessary to do the spectral purity check (that is useless for related compounds with similar spectra) in order to see that the shouldered rider peak on the second image is very likely to consist of two or more unresolved peaks.
5 posts Page 1 of 1

Who is online

In total there are 34 users online :: 0 registered, 0 hidden and 34 guests (based on users active over the past 5 minutes)
Most users ever online was 4374 on Fri Oct 03, 2025 12:41 am

Users browsing this forum: No registered users and 34 guests

Latest Blog Posts from Separation Science

Separation Science offers free learning from the experts covering methods, applications, webinars, eSeminars, videos, tutorials for users of liquid chromatography, gas chromatography, mass spectrometry, sample preparation and related analytical techniques.

Subscribe to our eNewsletter with daily, weekly or monthly updates: Food & Beverage, Environmental, (Bio)Pharmaceutical, Bioclinical, Liquid Chromatography, Gas Chromatography and Mass Spectrometry.

Liquid Chromatography

Gas Chromatography

Mass Spectrometry