-
- Posts: 3
- Joined: Fri May 11, 2018 10:12 am
- Location: Algiers
System suitability test FAILED
Discussions about HPLC, CE, TLC, SFC, and other "liquid phase" separation techniques.
6 posts
Page 1 of 1
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 ?
- tom jupille
- Site Admin
-
- Posts: 4978
- Joined: Wed Aug 11, 2004 4:55 pm
- Location: Alamo, CA / USA
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 ?
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
LC Resources / Separation Science Associates
tjupille@lcresources.com
+ 1 (925) 297-5374
-
- Posts: 3
- Joined: Fri May 11, 2018 10:12 am
- Location: Algiers
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%.
This is the summary of the technic results
And this is the graph of the sixth injection .
The retention time increased from injection 1 to injection 6 , and the RSD for this method is mentionned in the monograph =< 2%.
This is the summary of the technic results
And this is the graph of the sixth injection .
- tom jupille
- Site Admin
-
- Posts: 4978
- Joined: Wed Aug 11, 2004 4:55 pm
- Location: Alamo, CA / USA
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"
"403. That’s an error.
Your client does not have permission to get URL"
-- Tom Jupille
LC Resources / Separation Science Associates
tjupille@lcresources.com
+ 1 (925) 297-5374
LC Resources / Separation Science Associates
tjupille@lcresources.com
+ 1 (925) 297-5374
-
- Posts: 3
- Joined: Fri May 11, 2018 10:12 am
- Location: Algiers
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
https://drive.google.com/open?id=0BwJxH ... 01YWhueFB3
https://drive.google.com/open?id=0BwJxH ... xfRjVxU19n
and sorry again for being late
-
- Posts: 129
- Joined: Sat Nov 30, 2013 8:44 am
- Location: Belarus
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
Dmitriy A. Perlow
6 posts
Page 1 of 1
Who is online
In total there are 3 users online :: 2 registered, 0 hidden and 1 guest (based on users active over the past 5 minutes)
Most users ever online was 1117 on Mon Jan 31, 2022 2:50 pm
Users browsing this forum: Google [Bot], John Guajardo and 1 guest
Most users ever online was 1117 on Mon Jan 31, 2022 2:50 pm
Users browsing this forum: Google [Bot], John Guajardo and 1 guest
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.
- Follow us on Twitter: @Sep_Science
- Follow us on Linkedin: Separation Science