CBD Extraction Tek?

[adorno]

I browsed the forum a bit and couldn't find a thread dedicated to the topic of extracting the alkaloids from cannabis and isolating CBD. I understand that CBD is not psychoactive, but I also understand that it is said to have anti-anxiety, anti-psychotic, and perhaps even pain killing properties. For these reasons I think it would be a molecule worthy of more investigation. But perhaps it is nearly impossible to isolate without a lab? One thing that never fails to amaze me is that there aren't more teks involving liquid chromatography. The columns and the silica seem cheap enough, so why don't we use this process more often? Is it tremendously difficult to figure out or something? From what I understand, one would have to run a column if one desired to separate CBD from all the other cannabis alkaloids. But distillation could work as well, couldn't it?

I look forward to hearing all your thoughts about this. Could someone a little experienced in column chromatography maybe mock up a little tek for us, beginning with a hypothetical amount of hash oil and then running through the process of what solvents, silica, etc. to use? I'm not trying to get someone to do the work for us, I'm just hoping maybe someone more experienced could perhaps save us the trouble of having to learn all the chemistry behind chromatographic fractioning by giving us a simple step by step process instead. Or maybe someone could tell us how we might use distillation: the bp of THC is 157C, of CBD it is 180C, does that mean if I simply dissolved some hash oil in a solvent and distilled everything under 179C I'd be left with CBD? Probably not!

Again, CBD seems really interesting to me: a plant alkaloid with powerful anti-anxiety, anti-psychotic, pain-killing properties, Mary Jane without any of the freak out. I'm just really curious what that might be like and I can't imagine others aren't as well. So... If there are any tips someone more experienced than me might give I'd really appreciate them. Quality hash oil, though pretty easy to extract, isn't so cheap, and so it might be good to have some general idea as to how to extract CBD before putting quality hash oil on the line! Any thoughts?

 

[Cosmic Rift]

I'm nearly certain that a BHO extraction only extracts the THC (or extracts very little CBD). So you should be able to extract the THC from the bud leaving behind the CBDs. But I don't know of any way to extract pure CBD.

the bp of THC is 157C, of CBD it is 180C, does that mean if I simply dissolved some hash oil in a solvent and distilled everything under 179C I'd be left with CBD? Probably not!

No because theirs a big variety of different cannabinoids in the oil.

 

[adorno]

Thanks Cosmic... But in case I was unclear, I'm not so much interested in the other cannabinoids (CBN, etc.), but rather in Cannabidiol (CBD) in particular. My thought was, after extracting ALL the cannabinoids (including THC, CBN, etc.) using an old fashioned solvent pull, one could then take this residue and run it through a chromatograph and eventually isolate CBD. Or maybe one could do something very similar using distillation. I guess my question was whether you guys think it is even possible without a lab, seeing as how the cannabinoids are all so molecularly similar, and if so, where might one begin in order to do it?

And regarding the boiling point question, I agree, you're absolutely right, there are probably too many other things in the oil that boil off around the same temp as the CBD we're interested in, so that really only leaves chromatography. Let's say we have a column, then what do we do next? Is there a certain grade of silica one would have to use? Would the different fractions be visible in the column anyways or are cannabinoids completely clear? Is there any particular solvent or combination of solvents one should use to get the best results? etc. etc.

 

[Mitakuye Oyasin]

You might want to spend some time looking at and perhaps even asking questions to the folks on Project CBD Project CBD | Everything you need to know about CBD

There is also a very smart guy who goes by Morpheus at CRC Cornerstone Research Collective who might know some of the answers to your questions. Please post what info you find as I'm sure many here could benefit. I've heard, although I'm not sure it has been confirmed that industrial hemp is high in CBD and low in THC, so perhaps that might be one place to start. People in the medicinal cannabis communities are starting to grow low THC high CBD cannabis strains for exactly the reasons you list above. AFOAF has tried a few, one as high as 15% CBD and around 5% THC and it relaxed his back and neck muscles that has been very tense and relieved about 70% of the pain associated with both without having a particularly noticeable 'stoning' effect. They could still do work and function normally and more importantly operate an automobile, whereas an Indica that similar pain relief effects would not allow day to day work or driving a car (safely) for this individual.

I would like to see much more research done on CBD. Please let us know what you find out and I'll do the same.

 

[adorno]

Thanks for the tips Mitakuye, it looks like Morpheus is temporarily absent from CRC right now, but I sent the following email to Project CBD and I'll keep you all posted if and when they get back to me:

To Whom It May Concern,

I was wondering if anybody there at Project CBD might be able to help with some simple chemistry questions. You've sated that "the most practical, expedient, and reliable way to determine the effects of CBD rich Cannabis is to collect and analyze the data ourselves," and I could not agree more. With that in mind, I'm interested in extractions of CBD from cannabis using a liquid chromatography column, and I am having a difficult time finding information on exactly how to do this. Perhaps someone there could help. You see, most of the academic research papers on isolating or synthesizing CBD assume the availability of a professional laboratory, expensive equipment, and all sorts of "watched" or dangerous solvents, and so I was wondering if someone there might be able to suggest simpler tech for doing this. Specifically, let's say I have already extracted the oils and other various cannibinoids from my cannabis plant material. And let's say that I already have a column. What would one use for the stationary phase? (What mesh size, etc., ?) What widely available solvents (e.g., Bestine, Naphtha, Acetone, Ethanol, etc.) or combination of solvents would one use as a eluent? Will the different compounds present in the raw oils appear as fractions, or are they invisible naked eye? If there is anybody there at project CBD who might know the answers to questions like these I would really appreciate their help. Or perhaps someone there might put me in touch with someone else who could? Either way, even if someone simply told me that CBD extraction is impossible outside of a laboratory that would be nice to know. I'd just like some basic instructions on how to run a column on raw cannabis oils to get some /relatively/ pure CBD, or if this is even possible.

 

[adorno]

No word from anyone yet, and I'm sure this link has found its way to the Nexus before. But the following relevant information is contained there:

Extract the dried cannabis with a suitable solvent for several hours at room temperature or by refluxing. Filter through charcoal to clarify the solution, then chill overnight to precipitate waxes, then filter the solution again. Concentrate it to one-half volume, and extract it with 2% aqueous sodium sulfate (to prevent oxidation). Separate the aqueous layer, and strip the solvent. The residue is crude hemp oil.

The odoriferous terpenes can be removed by steam or vacuum distillation. Cautious distillation in vacuo yields a fraction of crude red oil (bp 100-220° C/3 mm). This can be purified by redistillation or column chromatography. Use ethanol to remove the residue from the flask while it is still hot. Filter the solution through charcoal, and strip the solvent. Distill the residue to yield pure red oil (bp 175-195° C /2 mm). Distillation must be stopped if smoke appears, indicating decomposition.

Because THC is heat-sensitive, it is preferable to isolate the cannabinoids by column chromatography. The simplest method of column chromatography is performed with ethanol and ether extracts of hemp on alumina, yielding two major fractions: (1) chlorophyll, CBD, and CBN, and (2) THC. A second, more difficult method is performed on Florisil (use 10 times the weight of the oil) with the solvent system hexane:2% methanol. This yields a doubly-concentrated, viscous oil which can be repeatedly chromatographed on alumina to separate the THC and CBD.

A few questions then:
Could something common be substituted for this "sodium sulfate"? (Or maybe that's easy/safe to make?)
What does "the simplest method of column..." mean? Does it mean the hemp oil is dissolved in some combination of ethanol/ether and then run through a column with alumina on the bottom [presenting two VISIBLE fractions, the first containing CBD, etc. and the second containing THC]? If so, then what /kind/ of alumina? And what might be substituted for the ether?

Either way, SWIM is not going to be able to try this experiment until sometime after December, but I thought I'd just throw this up now. I was also looking on ebay, and computer controlled HPLC systems are getting cheaper and cheaper. I mean, I know it is still allot, but one can find a complete HPLC system for like $2,000! The problem then, of course, would be figuring out how to safely/productively use it with little or no education in these matters!

 

[Mitakuye Oyasin]

Great job Adorno, please keep us posted as to your progress. Since Canada allows industrial Hemp and also tolerated cannabis and its research a lot more that the USA, perhaps you could look for labs or forums or groups there to help aid your search for info and techniques. You might also try forums like weedtracker and other similar ones as the members often ask and share information and techniques. Would love to have a selective extraction tech for CBD, especially from Hemp. Wishing lots of luck in finding good info. Peace

 

[Mitakuye Oyasin]

You might want to look into this patent. I think they have to post patent info online with the US patent office, so you might be able to find it and learn something from their process. Medical Marijuana Inc. Patent Pending Extraction - Cannabidiol (CBD) Possible Use In The Anti-Tumor and Anti-Cancer Nutraceutical and Pharmaceutical Industries.

 

[adorno]

This thread deserves an update. The topic does seem to arise every now again (e.g., here, and here, etc.).

SWIM reports that fractional/vacuum distillation of hemp oil is especially difficult. SWIM utilized several different setups: both microscale and 24/40, heating mantles and oil baths. These difficulties may have arisen because SWIM is a mere hobbyist and so overlooked something obvious. They may have arisen because cannabinoids have such high and relatively close boiling points. Either way, fractional distillation could not be accomplished by SWIM.

SWIM then developed some TLC plates (silica ~200 mesh). The eluents included: chloroform, acetone, and heptane. Of these eluents, the chloroform alone fractionated the oil, but the two fractions thus yielded (and exactly as described in the PDF linked on this thread) were THC and everything else (CBD, CBN, chlorophyl, etc.): useless, then, towards the goal of isolating of CBD. More experimentation could be done to find a better combination, but to SWIM's mind, once the task reached this level of calculation--if not well before--it was no longer practical to any wide scale application in kitchen chemistry.

On a side note, I have been interested in attempting fractional distillation of other essential oils and I am wondering if the difficulties faced by SWIM hold for every essential oil? Oil of Parsley Seed, for example, contains many interesting compounds; however, if I were to put some of this oil in a RB flask and attempt to fractionate it through a Vigreux column at ~25 mm would I run into exactly the same difficulties? Any insight into this question, or into what SWIM may have done wrong, would be greatly appreciated.

 

[MaNoMaNoM]

i had been looking into CBD a while, i hope it can be good for anxiety, and other stuff,
only the prices are unreasonable, and i suspect most of the sites are the same entity.

i've read hemp seed oil can contain small amounts of cannabinoids....
Hemp seeds themselves do not contain any, when they go threw the press process,
some plant fibers may be left on the seeds, so the plant cannabinoids go into the oil.
Lets say hemp oil only contains 1%, a gallon of oil should in theory yield 37.8 grams!
(1gram of CBD is currently going for about 300$$$!!!)

Here is a scientific analysis of hemp seed oil and it's cannabinoid contents.

Another possibility is unprocessed industrial hemp fiber.
There is hemp in China going for very reasonable prices.

It should be pointed out that the industrial process of fabric production does not affect CBD activity.The presented data suggest for the first time that flax products can be a source of biologically active cannabinoid-like compounds that are able to influence the cell immunological response. These findings might open up many new applications for medical flax products, especially for the fabric as a material for wound dressing with anti-inflammatory properties.
CBD is found in flax plant

In fact, flax is now part of an ever-growing list of plants that can produce cannabinoids (See image of Phytocannabinoid Producers).
Cannabinoids such as cannabigerol (CBG), cannabichromene (CBC), cannabicyclol (CBC), and cannabicitran (CBT) have been discovered in the following: species of rhodenderons (Rhodenderon Anthpogonoides), Voacanga Africana, liverwort (Radula Marginata), and woody umbrella (Helichrysum Umbraculigerum). Beta-caryophyllene is a cannabinoid present in virtually all plants and activates the CB2 receptor, notably it occurs in high amounts in cloves and black pepper.
Beta-caryophyllene is a dietary cannabinoid in many plants.

This is definitely worth some more research, and there is finally a good use for e-cigs!

 

[Chan]

Use your favourite search engine to look for "volcano poo"

Seriously.

The bp of the CBD compounds is above 200 C, so by vaping weed below 200 C, you get to enjoy a nice THC buzz, but CBD is left behind in the material.

Which you can then extract into oil or butter, with your usual method.

This is not GC, by any means, but for most folks, it's OK.