Measuring Nitrites in headspace

[MRiccio]

Hi,
Has anyone had success measuring Nitrite levels in the headspace of a package at 10-50 ppb level using GC? I myself am not an analytical scientist but supporting colleagues who are not on the exchange. Hoping to get them some valuable insights. I see others have inquired about testing in the drug product however this may be diff method required. We are stressing product at 60 degrees for a few days.

Thanks,

[Naiffer_Host]

Maybe this post can help as a starting point!

API seem to form N-nitrosamines upon oxidation (e.g. air) and without the presence of nitrosonium ions

In a recent public post, Moritz raised the following concern: I am currently looking at a very unusual problem, and am wondering whether a group member might be able to help: Some API seem to form N-nitrosamines upon oxidation (e.g. air) and without the presence of nitrosonium ions. For example Tolazamide was reported to form NHM upon oxidation. Is anyone aware of any regulatory guidance on such problems or has anybody experience whether such an oxidation can be supressed effectively by anti…

[MRiccio]

Thank you Naiffer. Yes good starting point. The detailed journal we do not have access to however our scientist can choose to purchase I think. I saw some info on oxidation but not Nitrite testing in headspace which has been tricky. Thanks for the support and reply.
Matt

[Yosukemino]

Hi, @MRiccio,

If you mentioned the ATNA, the following thread is helpful. And @Andrew.James will kindly help you. He is a professional in this field.

Automated Total Nitrosamine Analyser

Sample Preparation Some sample types can be added directly to the sample vial; others may require extraction into a solvent first. Once in the sample vial, the Reagent can be added, the vial sealed and then loaded into the autosampler. Automated Chemical Reaction Process The samples are vortexed and then heated. The chemical reaction causes the NO groups from any nitrosamines present to be released into the headspace of the vial. Headspace sampled The samples are allowed to cool to ensure…

[Andrew.James]

Thanks @Yosukemino for copying me in.

Hi @MRiccio

I have had a quick chat with our applications team. Direct GC headspace might prove very tricky from a sampling perspective. If it is nitrite levels in the packaging you are ultimately trying to determine then the ATNA system may be able to help. I think we would need to understand in a bit more detail what your hoping to do. If you and your team would like a chat to go over it and pick the brains of my apps team about what might be possible more than happy to put aside some time just let me know.