Spicing Things Up: BAM! LC/MS/MS Analysis of Synthetic Cannabinoids in Herbal Incense

I know it’s been forever since I’ve blogged, but at long last, I’m back on the radar!

Unless you’ve been living under a rock (and there’s nothing wrong with that), you’ve probably heard or read some news about herbal incense that’s spiked with synthetic cannabinoids. This incense can go by several names, including, K2, Spice, or legal pot. While some of the synthetic cannabinoids are controlled in some states, as well as being well on their way to DEA scheduling, other compounds in this large structural family are not yet controlled. When I say this is a large structural family, I mean that there are dozens of compounds that are actually members of a few different structural families that could be used to create ‘legal pot’. Since the purpose of this blog post is not to discuss the legal or moral ramifications of synthetic cannabinoids, let me get to the meat of the post: sometime in the near future (if not already), there may be a sizable demand for the testing of herbal incense products for a long and dynamic list of synthetic cannabinoids.

With that in mind (and because testing actual legal pot samples is fun), my colleagues and I at Restek – with the help of Paul Kennedy at Cayman Chemical – developed an LC/MS/MS method for a variety of synthetic cannabinoids in herbal incense. Here’s the good news: extracting and analyzing these compounds is pretty straightforward; the compounds chromatograph well, and although many of them share common fragments, hardly any of them are isobaric. Now for the bad news: new synthetic cannabinoids are coming out all the time; I did this work in December, and since then, some cursory internet searches have revealed several new compounds that have entered the market just in the past couple of months. Since most of these compounds are structurally related, chances are they’ll be as well-behaved as the compounds I’ve shown in my analysis, requiring very few method tweaks to add new compounds.

For further reading, check out the links below:

Press release from Cayman Chemical detailing collaborative work with Restek

Some interesting low-pressure GC work Jack Cochran did that included synthetic cannabinoids

12 Responses to “Spicing Things Up: BAM! LC/MS/MS Analysis of Synthetic Cannabinoids in Herbal Incense”

  1. Craig Brown says:

    We would be very interested in working up a method for these compounds in urine.
    The NLCP at RTI just published the results of their survey of certified drug testing labs, and many are testing for 2 or more of these compounds in urine. They are looking for metabolites in urine.

  2. Randall Edwards says:

    Hi Amanda – Good timing on your blog, I just got started on extracting spice from blood last week. I will have to try one of your biphenyl columns that you like so much!!

  3. Hi Craig,
    What a coincidence! I’ve actually already developed an LC/MS/MS method for a full panel of JWH-018 and JWH-073 metabolites in hydrolyzed urine. I actually did the work back in November, but I’ve been a little slow (okay, more than a little slow) getting the blog and the applications note out. I’d be happy to discuss it further with you. Also, stay tuned into the blog for more details on synthetic cannabinoids and their metabolites. I’m starting up some new work that will hopefully be really interesting.

  4. Hi Randall,
    It’s good to hear from you! Are you going to be looking for parent compounds in blood? I’m curious…do you know how long the parent compounds persist in blood? I’m not sure if there’s been much work done in that arena yet; most everything I’ve seen has been done in urine, but of course, all the research I’ve done has been for urinalysis anyway. I’d love to hear how the work turns out for you!

  5. Katrina Lindauer says:

    I was wondering if you can run this with the 3µm ultra biphenyl column instead of the 5µm? If so what would this change in your parameters and timing?

  6. Katrina Lindauer says:

    What are you doing to the urines to prepare them for injection on the LCMS?

  7. Since I ran this application with a relatively fast flow rate to begin with, you should be able to run the exact same conditions with a 3µm column as are shown for the 5µm column. Your peaks will be slightly sharper, and your backpressure will be higher than it would be with a 5µm column. The reason why I developed this method with a 5µm column is that larger-particle columns are less susceptible to clogging from biological matrix components than 3µm columns. Since the 5µm won’t clog as easily, you’ll get a much longer lifetime out of it. That being said, a 3µm column will give you sharper peaks, but like everything else in life, are always tradeoffs with chromatography.

  8. Hi again, Katrina!

    I’ve only analyzed incense blends for the synthetic cannabinoid parent compounds, but when I did the synthetic cannabinoid metabolites in urine, I simply did a 20x dilute-and-shoot (950µL mobile phase containing internal standard + 50µL hydrolyzed urine sample). If you’re running an instrument that’s less sensitive than an API 4000, you can do a high-pH (~10) liquid/liquid extraction, then dry down and reconstitute with mobile phase. These compounds are not volatile at all, so you don’t have to worry about losses during evaporation. For more details on extraction, feel free to email me.

  9. […] my last post back in February, I outlined an LC/MS/MS method for synthetic cannabinoids in herbal incense, and received some great comments. A couple of the comments were inquiries about a method for […]

  10. […] is analytical, and my colleague Amanda Rigdon has done some very good LC-MS/MS work on the analysis of synthetic cannabis and its metabolites in […]

  11. […] a Pennsylvania ban on both ‘bath salts’ and ‘spice’. Since I already have a couple of blogs on spice, I figured this time I’d blog a little bit about the work we’ve been doing on bath […]

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