Sunday, May 26, 2019

Solvency

OK, nothing to do with insufficient funds.  I've been experimenting with different solvents and decarbed MJ to see how the fluorescence depends on the solvent.  I don't have any photos (yet).  The table below summarizes my results to date.

Solvent                   Fluorescence color
Hexane                      Red
NMP                         Orange (has a yellow component)
N-Butanol                 Yellow-orange
DMF                          Red (not quite the same tint as hexane)
Propylene carbonate  Yellow-orange

NMP:  n-methyl pyrrolidone
DMF:  dimethyl formamide

All the solvents except hexane are polar, with a varying range of dielectric constants and dipole moments (most on the high side).  Water falls into this category, but cannabinoids aren't very soluble in water.  Cannabinoids do appear to be fairly soluble in hexane, NMP, n-butanol, DMF and propylene carbonate.  I also checked an ethyl alcohol tincture I made some time back, and it doesn't appear to fluoresce at all (it WAS made with decarbed MJ).  Time to try acetone to see how it performs.

The plant material I'm using for this particular set of comparisons has low to zero CBD content (just to keep things simple at this point).  So I don't know if CBD behaves the same or not.  I also don't know the concentration of all the other cannabinoids  this particular clone can contain, so that could be a complicating factor.

Ideally, there's a solvent out there that would produce different-enough fluorescent colors for CBD and THC to be able to distinguish them.  Examination of the molecular structures shows their main differences are on different locations on their molecules, compared to where their carboxyl group WAS (prior to being decarbed) -- so I'm not hopeful this approach will work for determining the THC:CBD ratio for a particular clone.  But it's worth some additional investigation .  The solvents I'm using are relatively inexpensive and available through Ebay or Amazon, and they're not excessively toxic (even ethanol is toxic, if exposure is too high).  Of course, it's a good idea to keep your exposure to solvents to a minimum no matter how "safe" they are claimed to be.  I use chemical gloves and good ventilation to avoid exposure.             

Saturday, May 25, 2019

Home-brew Cannabis potency analysis

Last year, due to an issue with improperly-marked marijuana plants, we ended up with some plants that had zero CBD content.  We are interested in the pain management properties of CBD, not getting high, so last year was a waste of our gardening time, water and garden space.  It was when I started looking into ways of doing my own analysis.  Sending material to a lab is expensive, particularly if you want to test a number of times to optimize your THC/CBD ratio (which depends on the "ripeness" of the buds).  My results, if successful, also could be helpful to others who are depending on getting the right "stuff" for their needs.

I started by looking at current mainstream methods.  Mainstream analysis techniques fall into several categories:  Gas chromatography, liquid chromatography, mass spectroscopy, and IR spectroscopy.  Thin Layer Chromatography kits can be purchased for home use, but they're not very good for quantitative work -- the size of a particular colored blob on the TLC plate is roughly proportional to the amount of chemical (THC, CBD etc.), but in my experience it was difficult to interpret the streaks on the plate.

While mulling over all these approaches, I did find a purely chemical way to at least tell you if your marijuana has some CBD in it.  It's pretty simple, too:  make up a 5% (by weight) solution of sodium hydroxide (A.K.A. lye) in ethanol or rubbing alcohol.    Put 100-200 milligrams of your decarbed bud in a glass vial and add the solution  at least halfway up the vial.  Screw on the cap and shake vigorously.  If the solution turns blue, your marijuana contains CBD.  The darker the color, the more CBD you've got.  THC doesn't turn blue.  With careful solution preparation and careful weighing it might be possible to get a quantitative measure of the CBD, but you'd need a spectrometer to tell you what the absorptivity of the solution is.  You can make a spectrometer using a web cam and DVD (for the diffraction grating).

I also discovered a paper that has a lot of information on cannabinoid analysis.  Its title:  "Chromatographic and Spectroscopic Data of Cannabinoids from Cannabis sativa L.", by Arno Hazekamp, Anja Peltenburg and Rob Verpoorte.  It turns out decarbed cannabinoids have a distinctive red fluorescence when illuminated by UV.  This may be the basis of a commercial THC analysis gadget that is currently selling for around $300 (pure speculation on my part).  The photo below shows three different samples I examined.  Two are decarbed bud and one is UN-decarbed.  Hexane is used as the solvent.


Pretty interesting.  While not shown, I also observed the same fluorescence in cannaoil made with coconut oil.  It glows a very pretty orange color, while pure coconut oil just reflects the purple color of the UV flashlight.  Cannaoil made with un-decarbed cannabis also doesn't glow orange.  The flashlight's peak output is specified to be at 390 nm.

The fact that the decarbed cannabinoids fluoresce suggests the mechanism is related to the site where the carboxyl group was (formerly) attached.  It's a benzene ring structure with an OH attached so technically speaking it's a phenol.  It would be nice if CBD fluoresced with a different color but at least the effect can be useful for a total cannabinoid test.

Searching the web, I found a thread on a MJ forum where the poster had noted the same thing.  The post mentioned some variability in the effect, comparing a commercial extract to a home-brew version.  I suspect the starting materials were different -- one was decarbed, the other, not.  There was speculation that the fluorescence was from chlorophyll, but as can be seen in my photo above, a chlorophyll-loaded UNdecarbed sample doesn't glow orange.  It's the vial on the right.


Monday, May 13, 2019

Spectrometer -- Useful for CBD/THC analysis?


The top spectrum shows the result for a high THC strain and the bottom shows the result for a high CBD strain.  A calibration procedure was used to compensate for variations in the illumination source (a 100 watt quartz-halogen lamp).  The color differences (as seen by eye) are mostly explained by the slight shift in the peaks centered around 625 nanometers -- the CBD color peak is slightly redder.

Conclusion:  I got a nice spectrometer to play with, but the idea of using Fast Blue B dye as a way to distinguish THC from CBD didn't work out.