Accurate, sensitive mass techniques required to identify specific peak of certain nitrosamines

Continuing its investigation into the presence of potential carcinogenic materials in various medicines, on May 28, the US FDA issued a fresh alert to patients and healthcare professionals about nitrosamine impurities findings in certain metformin extended-release (ER) products.

As the US FDA and other regulatory agencies continue investigations of nitrosamine impurities in drug products, scientific solutions providers like Agilent Technologies have devised sophisticated analytical testing tools which can be integrated into the drug discovery and development, and manufacturing and QC processes, to help manufacturers of APIs and formulations check for the presence and levels of NDMA across all processes.

Viveka Roychowdhury asks Samir Vyas, Director, Application Solution & Business Organization, Agilent Technologies for the long term learnings from the NDMA investigations, which have overshadowed the sector since 2018.

There could be a silver lining, as Vyas believes that once such analytical testing tools are adopted, manufacturers can constantly evaluate the drug quality and act to ensure related health safety before it reaches the marketplace. This will significantly reduce the burden on drug recalls and subsequent drug shortages, as well as prevent damage to drug manufacturer’s reputation and loss of business

As a major supplier of analytical equipment for the pharma sector, what are the solutions and services provided to API and formulation manufacturers to help them check for presence and levels of NDMA?

In 2018, traces of nitrosamines like N-Nitrosodimethylamine (NDMA) were found in some sartan (ARBs) and ranitidine drugs, which instigated several market recalls. Also, detection of these nitrosamines in other classes of medicine, such as ranitidine and metformin, raised additional health concerns for regulators globally. The US FDA makes it clear that pharma drug manufacturers are responsible for understanding their processes, which includes preventing the presence of such unacceptable impurities. Manufacturers are also responsible for developing and using suitable methods to detect and limit these unacceptable impurities, including any new impurities that may arise when they make changes to their manufacturing processes.

The US FDA and other regulatory agencies enforced even more stringent regulations for the evaluation and testing of nitrosamines (e.g. NDMA) in drugs. Regulatory agencies around the world, such as the US FDA, General European OMCL network and others published analytical testing methods using Agilent’s single quadrupole GC/MS, triple quadrupole GC/MS, Q-TOF & triple quadrupole LC/MS to reliably detect and quantify NDMA in ARB and ranitidine drugs respectively.

As a major supplier of testing equipment to the pharma industry, we verified the regulatory procedures on both our GC/MS and LC/MS technology to give confidence to our customers.

We also developed a single LC-MS/MS method for simultaneous analysis of 12 such nitrosamine compounds (e.g. NMBA, NDE) in active pharmaceutical ingredients (APIs). We also considered various formulation/matrix types to ensure that our solution helps the formulation manufacturers as well. Moreover, in India, digital platforms, such as webinars have helped us to magnify our outreach and spread awareness about best analytical practices among our customers.

Agilent offers comprehensive LC/MS and GC/MS solutions with excellent sensitivity, repeatability, accuracy and precision with regard to analysis of multiple nitrosamines. The results not only meet but outperform the regulatory requirements, for confident NDMA and other nitrosamine impurities testing. Furthermore, power of innovative analytical technology, guided workflow and software libraries are helping our customers to analyse the entire product lifecycle and define the root cause of genotoxic impurities.

The pharma supply chain is today more global than it was earlier. How will pharma companies manage continuous risk evaluation, quality testing, verification of suppliers, etc. Beyond the NDMA issue, what are the long-term learnings?

With evolving pharma globalisation, the regulations are getting more stringent. Regulators are constantly working towards global harmonisation of standards to conform drug quality and compliance requirements. The recent worldwide drug recalls for ARB and ranitidine based products amplified the reliance on the sensitive mass spectrometry tools to confidently detect previously undetected trace level impurities and enabled even more stringent regulatory requirements to ensure drug quality standards.

Regulators are asking manufacturers to review their manufacturing processes to identify and, if necessary, mitigate the risk of presence of nitrosamine impurities. Multiple steps have been proposed and the European Medicines Agency (EMA) encourages manufacturers to submit the outcome of risk assessments before October 1, 2020.

When developing analytical methods, many technical aspects require evaluations. For example, potential interferences caused by the presence of trace amount nitrosamines in the testing materials utilised (e.g. water, airborne sources, plastics products, etc.) and in situ formation of nitrosamines. Hence use of accurate and sensitive mass techniques are required (MS/MS or Q-TOF) in order to overcome interferences in the identification of the specific peak of a certain nitrosamine (e.g. DMF co-eluting with NDMA).

In the long run, with the adoption and integration of such sophisticated analytical testing tools into the drug discovery and development, and manufacturing and QC processes, the manufacturers can constantly evaluate the drug quality and act to ensure related health safety before it reaches the marketplace. This will significantly reduce the burden on drug recalls and subsequent drug shortages, as well as prevent damage to drug manufacturer’s reputation and loss of business.

CarcinogensEMAMetforminNDMAnitrosaminesranitidinerecallssartansshortagesUSFDA
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