A significant amount of time and money must be invested into the registration of a crop protection product. The chance of a discovery compound passing all the many safety and efficacy tests on the way to market is about 1 or 2 in 100,000 and, on average, it can take 8–10 years and around US$ 260 million before commercial launch.

As senior analytical chemist at Syngenta, Dr Kirt L. Durand is responsible for quantifying nitrosamines in technical material for

use in pesticides, herbicides and other crop protection products. Nitrosamines are formed by reaction of secondary or tertiary amines with a nitrosating agent.

Syngenta must verify the absence of nitrosamines or quantitate the amount of nitrosamines (ppm levels) in their active ingredients, showing they are below acceptable limits, to be able to commercialise them and ship them around the world.

For every new compound that has the potential for nitrosamines, Dr Durand develops methods to ensure their levels are acceptably low. Detection technology for this specific need had not advanced from the early 80s until recently.

The Thermal Energy Analyser (TEA) was being used by Syngenta, prior to it being bought by Ellutia Chromatography Solutions from Thermo Fisher Scientific. Ellutia identified the drawbacks of the existing instrument and developed a new version that would meet Syngenta’s analytical needs and those of other similar players.

Drawbacks of previous analytical systemThe TEA 502 and 510 systems were first produced in the 1970s by Thermedics. These versions had an LC injection and GC injection mode and stood about the size of a refrigerator. The successor to these first generation instruments – the TEA 543 and 610 versions – only offered the GC injection mode. This technology changed hands several times and ended up with Thermo Fisher Scientific, before being acquired by Ellutia in 2006.

Dr Durand outlines some of the drawbacks of the legacy system:

“Productivity was not good. Not only was the system constantly down, it became impossible to get parts for it. With the instrument regularly down and difficult to repair, samples which should take a couple of days, were taking us weeks. This hampered our ability to register materials and get to market quickly.

Syngenta uses new generation TEA by Ellutia to accelerate speed to marketSyngenta provides products and solutions to help farmers achieve global food security for a growing population, sustainably. According to the company, without crop protection, around 40% of the world’s food would not exist. The crop protection industry is one of the most highly regulated industries in the world. The registration of a product requires demonstration of safety for workers, for all aspects of the environment, for the crops that are being protected and for the food that is eaten. Sophisticated risk assessments are made based on data from hundreds of safety studies and an

understanding of Good Agricultural Practice.

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Sensitivity was not optimum and we could only run about 3 injections before having to stop, flush and calibrate. Safety was also a concern. As the old system contained an ozone trap, ozone was held in place and any failure of an O-ring or part of it could run the risk of toxic ozone leaking into the lab.

It was imperative for our business to find a better solution. Luckily, Ellutia delivered for us!.

Maintenance, while challenging, was also very messy! The oil pump the system used had to be refilled with new oil very regularly due to the ozone in the trap corroding the oil, turning it into messy sludge, rendering the system difficult to clean and re-lubricate.

The only alternative system available was a NOx analyser, however, that gives no option to hook up with chromatography, giving you only total NOx levels in one peak. We needed to be able to separate out the nitrosamines for more detailed analysis.

It was imperative for our business to find a better solution. Luckily, Ellutia delivered for us!”

The next generation TEA 800The result of several years of research and development is Ellutia’s TEA 800 series. The TEA 800 Series was designed with input from users of older model TEA’s to ensure this model delivered what customers demanded. The redesigned TEA was smaller, easier to service and simpler to operate, whilst not compromising on the analytical performance of its predecessors.

However, Syngenta required a completely bespoke version of the TEA, as Phillip James, Ellutia’s managing director, explains:

“Since the acquisition of the technology, our main focus was on the vast majority of TEA users with GC-TEA applications and we had not ventured into the LC-TEA applications supported by the first generation TEAs.

However, Syngenta required the system to be LC compatible, as moving to GC would have meant redeveloping existing methods and this was not an option. We used our extensive technical capa-bilities to develop a new LC-TEA to meet their needs and solve all of the challenges of the previous system.”

Benefits of the TEA systemThe standard 800 Series TEA, includes a number of benefits, as listed below:

• High selectivity for nitro, nitroso and nitrogen (when operating in nitrogen mode) which allows only the compounds of interest to be seen and the others ignored.

• Very high sensitivity <2pg N/sec Signal to Noise 3:1 which means it is able to detect compounds of interest down to extremely low level.

• It has a range of interface options, meaning it is compatible with most GC’s manufacturers and models.

• Includes an external vacuum pump, which saves bench space and makes servicing simpler and easier.

“There is no calibration or fine tuning required, it’s pretty much a press a button and go.”

The Customised LC version, developed for Syngenta, delivered numerous benefits, including using a different interface with a furnace rather than the standard pyrolyser, to allow for the additional energy required and larger diameter tubing for working with a liquid sample rather than a gas. This is further described by Dr Durand:

“The new system enables us to run 5-6 times more samples and is much more automated than the previous one. There is no calibra-tion or fine-tuning required, it’s pretty much press a button and go!

The footprint of the system is much improved, freeing up valuable space in our lab. “

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Featuring an ozone destroyer, the system eliminates the safety risk of ozone leaks and the dry spiral pump requires no oil change or maintenance, just a simple filter change about once a year.

“We have seen significant productivity gains, reduced costs on maintenance and more accurate results.”

Working with EllutiaThe bespoke TEA, designed for Syngenta, was developed by Ellutia’s technical team in the US, headed up by Adam Zapiecki. While talking about the relationship with Ellutia and service they provided, Dr Durand commented:

“We have seen significant productivity gains, reduced costs on maintenance and more accurate results.”

“Ellutia provides excellent customer service. Adam was always available and on hand to help troubleshoot the previous system and was incredibly proactive in proposing the new system espe-cially to meet our needs. The development of the system went smoothly, as did the set up and installation and we couldn’t be happier with the end result. We have already bought a system for our manufacturing plant and I am keen to transfer all of our global NOx systems over as soon as possible.”

“The development of the system went smoothly...and we couldn’t be happier with the end result.”

Andrew James, Ellutia’s Marketing Director commented: “We pride ourselves on our close relationships with customers and regularly deliver customised solutions to meet individual needs – something rarely offered in our markets. In the case of Syngenta, our technical manager serving the US market, Adam Zapiecki went above and beyond to develop a new system, the technology for which had not been upgraded for decades. We are delighted with the outcome, which is genuinely a revolution in TEA detection and is totally unique in the market.”

The Ellutia 800 Series TEA detectors are able to quickly identify and analyse N-Nitro, N-nitroso and Nitrogen containing compounds. Application areas include explosives analysis as well as Nitrosamine testing in rubber, toys, water and food. Ellutia offers accessories such as the Thermosorb-n air sampling cartridge for monitoring airborne Nitrosamines and the chemical stripping glassware system for total Nitrosamine analysis.

To learn more about Ellutia visit www.ellutia.com , call us at +44 (0) 1353 669916 or email us at info@ellutia.com

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UK Tel: +44 (0)1353 669916 Fax: +44 (0)1353 669917USA Tel: +1 843 259 2307Germany Tel: +49 (0)561 400 0430 Fax: +49 (0)561 400 0429Email: info@ellutia.com Website: www.ellutia.com

For more information about Ellutia please visit https://www.ellutia.com/, call us at +44 (0) 1353 669916 or email us at info@ellutia.com.

ELLUTIa_Case_Study_Syngenta.indd 4 22/02/2018 14:44