System suitability test FAILED

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

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Hello, i launched the USP technic dedicated to Azithromycin tablets organic impurities dosage. The System suitability solution were injected six times , unfortunately the RSD for Area were higher than the 2.0% mentionned (3.6% for azithromycin related compound F , and 13.4% for desosaminylazithromycin) . The case is that the fifth injection were shifted to the right and weren't stackable with the others . Any suspected reason for that ?
I can think of many possible reasons, but the fact that you saw a retention time change on one of the injections suggests a flow rate problem. One possibility is that the one bad injection is the cause of the high RSD (what does the RSD look like for the remaining 5 injections?).
Also, is there a trend in the response (in other words, is the high RSD coming from a gradually increasing or decreasing response rather than random variation)?
Have you seen acceptable RSD with other methods run on this system ?
-- Tom Jupille
LC Resources / Separation Science Associates
tjupille@lcresources.com
+ 1 (925) 297-5374
Thank you for answering .
The retention time increased from injection 1 to injection 6 , and the RSD for this method is mentionned in the monograph =< 2%.

Image
This is the summary of the technic results

Image
And this is the graph of the sixth injection .
Unfortunately, the images you linked to are not accessible. Error message was:
"403. That’s an error.
Your client does not have permission to get URL
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-- Tom Jupille
LC Resources / Separation Science Associates
tjupille@lcresources.com
+ 1 (925) 297-5374
Sorry it was my mistake , here are links to access to the pictures on google drive

https://drive.google.com/open?id=0BwJxH ... 01YWhueFB3


https://drive.google.com/open?id=0BwJxH ... xfRjVxU19n

and sorry again for being late
Hello. As far as I see it seems to be an integration issue. Try to tweak integration options and reprocess your data or try manual integration.
Best regards,
Dmitriy A. Perlow
6 posts Page 1 of 1

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