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Testing & Processing Cannabinoid analysis, Classification, Extraction

Fake It Till You Vape It?

Despite the lack of information around their safety, e-cigarettes and vaporizers containing hemp-derived delta-8 THC continue to rise in popularity. A number of studies have cast doubt on the lab testing of these products (check out our feature with Chris Hudalla for more on the elusive delta-8 THC “unicorn”); few would disagree that more data on the health and safety implications are needed.

To dig into the issue a little deeper, Irfan Rahman and Jiries Meehan-Atrash from the Department of Environmental Medicine at the University of Rochester, New York, analyzed 27 products from 10 brands using a combination of nuclear magnetic resonance spectroscopy (NMR), gas chromatography-mass spectrometry (GC-MS), and inductively-coupled plasma-mass spectrometry (ICP-MS). What did they find? None of the products they analyzed showed accurate delta-8 THC labeling. On top of this, all of them contained reaction side-products (including Δ9-THC), heavy metals, and a previously undescribed cannabinoid – and 11 had unlabeled cutting agents (1). We spoke to Irfan and Jiries to find out more.

What was the motivation behind your research? 
 

New products emerge on the vaping market all the time, but large trends like delta-8 THC aren’t as frequent. In the shadow of the e-cigarette or vaping use-associated lung injury (EVALI) outbreak, we felt it was something that needed to be investigated further. EVALI is a lung disease caused by e-cig/vaping and known to be associated with THC products including vitamin E acetate and other toxicants. The fact that these products are of synthetic origin is doubly interesting. 

Could you elaborate on the analytical approaches you used in the study? 
 

We primarily used 1H-NMR spectroscopy because of its proven utility for characterizing natural products, and Jiries’ research background involved developing NMR methods for the analysis of e-cigarettes. NMR offered fantastic insight into the major components of the e-cigarettes and vaporizers in an omics sense, which uncovered further details about the origins of some products. When we added GC-MS and manual column chromatography to the toolbox, we were able to account for nearly all the components in each product.

Can you walk us through the main findings?
 

The main finding was that the reported lab test values were all inaccurate –  likely due to a lack of optimization in the HPLC-UV methods used by the various labs for testing. We also found a number of unlabeled additives, such as triethyl citrate and medium chain triglyceride oil – this was concerning, but not particularly surprising. What was particularly striking was the diverse mix of cannabinoids in the products. Someone consuming traditional cannabis would not be exposed to these, and we simply have no idea what impact they might have on the brain or respiratory system.

People that use delta-8 THC vaporizer (or those curious) should take these findings as a stark warning. Do you really want to inhale something when you aren’t totally sure what’s in there? Our study also highlights the potential problems with the existing cannabis lab-testing infrastructure; if regulators don’t enforce strict certification of testing labs, policies around product potency and composition won’t be enforced.

You also identified a new cannabinoid… Please tell us more!
 

Several interesting signals in the 1H-NMR spectra of all the delta-8 THC vapor products suggested the presence of many cannabinoids other than delta-8 THC, so manual column chromatography was used to fractionate the sample. One fraction had a peculiar 1H-NMR spectrum in that it contained an isopropyl group, but it still displayed the 21 signal on the 13C spectrum, meaning it had to be isomeric with THC. After many 2D experiments and GC-MS, which are all available for viewing in the supporting information, a structure was proposed and confirmed. A scifinder search shows that a similar structure was proposed in 1975 by a group in Milan, Italy. However the structures were not named, and they lacked the double bond. This is the first full characterization of a tricylic cannabinoid that contains an isopropyl group.

What are the next steps for your research? 
 

Working on cannabinoid products presents many regulatory challenges, but we must be vigilant about emerging trends. We hope that policies at the federal level loosen for academic institutions in the future, and that funding opportunities become available for this emerging field. In terms of next steps, there are several THC isoforms that are sold in the market as a vaping product. We would like to analyze the chemistry, toxicity, and human health effects of these products.

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  1. J Meehan-Atrash and I Rahman, Chem Res Toxicol, 35, 73 (2022). DOI: 10.1021/acs.chemrestox.1c00388
About the Author
Lauren Robertson

By the time I finished my degree in Microbiology I had come to one conclusion – I did not want to work in a lab. Instead, I decided to move to the south of Spain to teach English. After two brilliant years, I realized that I missed science, and what I really enjoyed was communicating scientific ideas – whether that be to four-year-olds or mature professionals. On returning to England I landed a role in science writing and found it combined my passions perfectly. Now at Texere, I get to hone these skills every day by writing about the latest research in an exciting, creative way.

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