In the hunt for a Nitrosamine Universal Method?

Our team is working on a new initiative to support the Nitrosamine Exchange community! We are considering building a repository of Analytical Methods developed and validated for Nitrosamines Impurity testing. The repository can potentially be populated with reviewed methods donated by our community members.
While most published methods are intended for API or Drug substances, we feel the need to have analytical methods that have been developed, validated, and use for different matrixes.

Any thoughts? What would be the most valuable feature in this repository of analytical methods for you? Does the novel ring a bell?

@trust_user_a @trust_user_b

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Buen día

Yo considero que lo mejor seria hacerle como se hace con las impurezas, es decir, se fija una especificaición y todos la debemos de cumplir tanto para conocidas, desconocidas y totales y todo debera ser analizado por masas.

Así cualquier cosa que te salga simplemente la elaluas y ves en que criterio entra y si puede pasar o no, es decir si cumple o no cumple, apruebas o relachazas, come hace por ICH Q2a o b.

这是一个非常棒的想法。杂质只要没有超标的风险,就不会纳入药典各论或通则。本数据库可以发挥一个亚硝胺杂质检验的专门讨论平台,通过各捐献人捐献行动丰富我们亚硝胺杂质检查知识,包括不会纳入药典各论或通则的方法的讨论,其优势在于:1、专注于亚硝胺检验方法细分领域;2、在这个细分领域较药典论坛内容更丰富。

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Continuing the discussion from In the hunt for a Nitrosamine Universal Method?:

Hello Naiffer
Screening methods for Nitrites.pdf (579.6 KB)

This is very good initiative and appreciate you taking this up.

Given that nitrosamines need to be worked at very low, read, trace level concentrations, you need highly sensitive, complex and specialized instrumentation and not to mention orthogonal methods as all potential nitrosamines may not be detected and estimated by one method.

As an alternative we could look at testing for Nitrites, universal precursors to most nitrosamines.

There’s an excellent paper published by J. Jires and M Dousa which employs a simpler and more rapid UPLC-MS method, a chromatographic run time of around 4 minutes and LOD about 0.005 ppm. Apparently, this method should be suitable for routine QC testing as well.

Considering the reaction rate of N-nitrosation is 2 with respect to nitrites, controlling nitrites should significantly reduce the levels of nitrosamines.

Here is the link to “Nitrites as precursors of N-nitrosation in pharmaceutical samples – A trace level analysis”: https://www.sciencedirect.com/science/article/pii/S073170852200098X

Regards
Pearl

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Gracias @GabrielAlvarado por tu comentario. Dado la multitud de fuentes de estas impurezas y lo especifico de las condiciones para que se puedan formar, considero que el modelo de aplicar un listado de impurezas y definir una especificación no es viable en este caso. El modelo de análisis basado en riesgo es el modelo idóneo a utilizar (ha sido la tendencia en ICH Q3D con Impurezas Elementales). En corto, si un fabricante demuestra que sus procesos, ingredientes y condiciones de fabricaciones no generan riesgo de formación de Nitrosaminas, NO entiendo la necesidad de obligar a realizar analisis de Impurezas de Nitrosaminas.

@daixulin thanks for the comment and feedback. The team thinking through this initiative is to provide a first stop for anybody looking to develop their product-specific analytical method. There are great success stories of this type of data-sharing effort.
Just to be clear this initiative is taking place outside the compendial space and separate from any activity or work happening in the pharmacopeia standard development.

@Pearlp that’s exactly what we are trying to do here… we will need feedback and information on all those ‘novel’ methods that prove to work well from our community members!

Great initiative! We can upload the Agency’s recommended API specific methods wherever available for e.g. N-nitroso varenicline by FDA.

By the way, could you please share the link of nitrosamine presentation by Dr. Raphael Nudelman.

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@Naiffer_Host

Please ignore earlier request. I got the presentation by Dr. Raphael. Thanks.

It is an great initiative and would be great, as industry pools / contributes the methods.

Ad-hoc projects of the OMCL Network - European Directorate for the Quality of Medicines & HealthCare?

https://www.fda.gov.tw/ENG/siteList.aspx?sid=10360

https://www.canada.ca/en/health-canada/services/drugs-health-products/compliance-enforcement/information-health-product/drugs/angiotensin-receptor-blocker.html#a4

Hi,
we´ve multiple methods for Nitrosamine analysis. I can post the PDFs for the technotes, but first I would like to have the approval of Naiffer for this because they´re all on the base of SCIEX instruments. In any case, I can send the methods in private if needed.
BR

We will share soon the mechanism for submitting ideas and potentially donating methods for this repository! Stay tune…

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