Botanical Dietary Supplement Screening using NMR and MS

insights from industryKim ColsonBusiness Development ManagerBruker Biospin

An interview with Kim Colson from Bruker Biospin, discussing the applications of NMR and mass spectrometry in the field of botanical science and her recent presentation at the European Nuclear Society.

First of all, can you say a few words to introduce yourself?

My name is Kim Colson. I’m the Business Development Manager for Bruker Biospin, and right now my group is focusing on the botanical and herbal products and dietary supplements industry and bringing new tools to that industry that will help to meet their needs for quality control assurance.

Soil analysis - a photo by Rattiya ThongdumhyuRattiya Thongdumhyu | Shutterstock

Can you give a brief overview of the work on botanical analysis that was presented at the Bruker symposium at ENC 2014?

Jim Hamly presented a very nice piece of work that he’s been doing on the development of new analytical approach towards the identification of black cohosh. Black cohosh, or Actaea racemosa, is a botanical material that’s harvested and sold in the dietary supplement industry.

Jim’s work was to identify a new NMR and mass spectrometry approach towards distinguishing the very closely related species of this material, and he highlighted the different strengths of MS and NMR for that purpose. Mass spectrometry, of course, is a highly sensitive technique, and NMR brings really high reproducibility, and the ability to quantify the particular metabolites within the material.

Black cohosh root herb used in natural alternative herbal medicine over old wood background.marilyn barbone | Shutterstock

Why is material identification such an important process in the food and supplements industry?

There is a very large increase in the sales of dietary supplements and herbal products going on right now worldwide, and it’s over a 20 billion dollar business at this point in time. This has caused increased concern about adulteration, particularly of those materials that are very high-cost materials to produce.

Adulteration is a safety concern to consumers, of courseconsumers need to know what they’re actually purchasing when they’re purchasing the dietary supplement. As a result of these concerns for safety, there was a ruling that was put in place in the year 2010 which has required the current manufacturing processes to include a quality assurance on all of these materials, and of course that’s going to mandate testing on these materials to identify the species of botanical that’s in these products.

How do Bruker’s NMR products enable customers working in this field?

Bruker sells NMR products to assist in the identification of these botanical materials and quality control of dietary supplements. The systems that we provide can be customized for specific materials – that means that the customer who doesn’t have NMR knowledge can run the system in complete automation and get NMR data.

The system provides reports which validate that the material meets the product expectation, as defined by the producer, and it also quantifies the key metabolites. Bruker also provides services to assist the customers in customizing the instrumentation - and of course we provide training to get people up to speed on how to run an NMR, if they also want to go in to more detail so that they can customize their own system for different sorts of analysis.

Botanical Dietary Supplement Screening

What is it about NMR that makes it such a useful tool for analysis of botanical materials?

There are several components of NMR that makes it extremely valuable for this. One is high reproducibility - NMR is extraordinary with regard to its reproducibility.

What that means is I can take a sample, acquire the data in my lab, and you can take that exact same sample and acquire that in your lab and we will get identical results. That allows us to share information with each other, and share analysis so we know that we’re getting very high quality control on our material in each laboratory. Combining data from multiple labs allows us to get the identity of the botanical or dietary supplement that we’re looking at, it allows us to detect details like the growing location, the health status of the plants that were harvested, or even what time of year the material was harvested at.

So we can get a tremendous amount of information, and that all comes from that reproducibility of the NMR spectrometer.

Additionally, NMR is a compound specific technique. That means I can identify all the compounds that are present in the material and that’s very powerful information. NMR is an absolutely quantitative technique, so I can determine the amount of each key component. That assists someone then in defining the strength of their dietary supplement or their botanical material, because many of the key components are associated with the materials benefits.

Please tell us a little bit about the poster that you presented at ENC.

The poster that we presented at the ENC was about some work we did on quality control of botanical material, using a 400 MHz instrument similar to the one beside me here, our Assure raw material screening product. That product allows you to acquire the data, analyse it, and report the material quality in full automation.

For this work, we tried to find materials that are commonly adulterated. Some of the most common adulterated materials in the herbal products industry are related to weight loss products.  So when we hear of a weight loss product that’s been recalled by the FDA, we go online and we buy as much of the stuff as we possibly can, so then we learn how to detect the adulterates in those particular materials.

In the poster, we present a bee pollen, which is claimed to be an all-natural herbal supplement, but in reality it contained a drug material called Sibutramine, which was recalled as a product a number of years ago because it has toxicity. Also in that same material we found phenolphthalein, which was used for centuries as a laxative.

So the combination of this drug and this laxative is what has actually caused the efficacy of this bee pollen product. Of course, it is therefore not “all-natural” as was claimed on the label of the ingredients, so the consumers that bought this did not know that they were buying two materials that were no longer used for various reasons.

The other case that we’re presenting in this poster is a non-targeted approach to analysis, looking at mixtures in mixtures. The example we used was borage oil. The borage plant is highly expensive, making borage oil very expensive too. Like most expensive products, borage oil has been subject to adulteration, in this case by sunflower oil.

In this analysis, we spiked a bunch of borage oil with different amounts of sunflower oil, to determine what level of sunflower we could detect, using a non-targeted partial least squares approach.

This gave us a very rapid way to say that a material is not 100% borage oil, but instead contains a small amount - less than 1% - of sunflower oil.

What is your vision for how this work will be applied in industry in the future?

This is definitely going to be used in the quality control area of industry - manufacturers will be able to use this to meet the Good Manufacturing Practices rules in quality control assessment of their materials.

This will also help purchasers, because purchasers then can make better informed decisions about the material that they’re purchasing. Knowing the exact species of the material will help them ensure high quality, high strength, good composition and good purity.

This approach is not going to be limited to quality control – it will also help governments in detecting adulteration, and it will assist with research and development, allowing people to monitor their product development so that they can enhance the efficacy or performance that they want from the product.

Consumers will also benefit from this, because there will be more safety within the botanical and dietary supplement industry, and that is of course a very great benefit to all of us who utilize those products.

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