[SkyHighLer]

^^

"CHAPTER 3

Preparative isolation of cannabinoids from Cannabis sativa by centrifugal partition chromatography
•••
Arno Hazekamp, Ruud Simons, Anja Peltenburg-Looman, Melvin Sengers, Rianne van Zweden, Robert Verpoorte
••
Leiden University, Department of Pharmacognosy, Gorlaeus Laboratories Leiden, The Netherlands
•
Published in J. Liq. Chrom. Rel. Technol. 2004, 27(15): 2421-2439

Abstract
A simple method is presented for the preparative isolation of seven major cannabinoids from Cannabis sativa plant material. Separation was performed by centrifugal partition chromatography, a technique that permits large scale preparative isolations. Using only two solvent systems, it was possible to obtain purified samples of the cannabinoids; (-)-∆9-(trans)- tetrahydrocannabinol (∆9-THC), cannabidiol (CBD), cannabinol (CBN), cannabigerol (CBG), (-)-∆9-(trans)-tetrahydrocannabinolic acid-A (THCA), cannabigerolic acid (CBGA) and cannabidiolic acid (CBDA). A drug-type and a fiber-type cannabis cultivar were used for the isolation. All isolates were shown to be 90-95% pure by gas chromatography. This method makes new cannabinoids available on a large scale for biological testing. The method described in this report can also be used to isolate additional cannabinoids from cannabis plant material."

https://openaccess.leidenuniv.nl/bit...297/Thesis.pdf

[goose920]

Pangea- those are amazing!! I really need to give this method a try. Been reading up about it on here all day and I think I could. I have a couple questions I haven't seen asked and I hope it's not because they are silly! :-p

[SkyHighLer]

I used to have an Acme 6001 stainless steel centrifugal juicer, seems to me it might be useful for experimental purposes. Either to spin up some high THC-A laden oil to see if the THC-A crystals can be coaxed out, or to do some on the cheap centrifugal partition chromatography by packing the screened basket with your filter material, and squirting measured amounts of solvent into the spinning basket at intervals.

It can be operated with the top off as can be seen in this video,

https://youtu.be/LvBoQNVaLJI

You should be able to wash down the individual partitions with some extra solvent from a lab wash bottle while keeping it running. The switch is the only source of ignition, tape it in the on position, and switch it externally.

You could probably also use it to filter winterized oil, by pre-freezing the basket lined with filter paper.

Pic of the basket

[SkyHighLer]

^ Used SS Acme 6001's are cheap at eBay, they're extremely robust, should do you fine, but it's still available under the Waring Commercial brand,

https://www.amazon.com/6001-Juicerat.../dp/B0028RXDFM

At that page I noticed they have filter strips to line the basket,

https://www.amazon.com/Replacement-F...PDXC7JS3CJHJJG


You might want to slow it down, should function fine with a 120V 10A or higher rated Variac, also something you might consider getting used,

https://www.amazon.com/Circuit-Speci...le+transformer

If you run it with the top off, use some tape or bungee cords, whatever, to hold the collection pan more firmly in place, you don't want the spinning basket scraping against the pan when working with flammable solvents. I say that because I just know someone's going to try filtering sub zero butane through it, just covering my ass.

[weedaholic721]

Talking gibberish there SkyHighler I see.

But seriously, you might be in to something good. It would be great for all the the high terpene extractions goin around. The cannabinoids naturally separate it seems so it seems like a very good route for getting as much if the terpene layer off of the cannabinoid microcrystals.

[SkyHighLer]

^ All kinds of things you could try with it, how about thickly packing the basket with "acid-washed see-sand (Sigma) and topped with glass pearls (±1 mm diameter)?"

"3.2.7 Separation of acidic and neutral Cannabinoids

A glass-filter (mesh size 2) of about 5 cm in diameter and 7 cm in height was filled for 2/3 with acid-washed see-sand (Sigma) and topped with glass pearls (±1 mm diameter). Before use the sand was sequentially washed with 200 ml of hexane, ethanol and water. Cannabis hexane extract was concentrated to about 5 ml of hexane, placed drop-wise on top of the sandfilter and evaporated by using a warm air blower. The sandfilter was then placed onto a suction Erlenmeyer and acidic cannabinoids were eluted by washing the sandfilter under vacuum with a 0.1 M NaOH solution. The elution was continued until the eluate turned from deep-orange to colorless. Neutral cannabinoids and other compounds were then eluted with ethanol (200 ml), followed by hexane (200 ml). Acidic cannabinoids were precipitated in the aqueous eluate by adding HCl until the pH reached 2 and then filtered through the (dried) sandfilter. The precipitate that remained on top of the sandfilter was finally eluted with ethanol (200 ml). Neutral and acidic cannabinoid fractions were both concentrated into a small volume by evaporation under reduced pressure and analyzed by GC and HPLC."

https://openaccess.leidenuniv.nl/bit...297/Thesis.pdf

[SkyHighLer]

^^ You could even do the initial extraction with an Acme SS centrifugal juicer:

1) Line the basket with a couple of the filter papers I linked to above, wet them with solvent.

2) Grind your herb through the machine like you would fruit or vegetables.

3) (optional) Freeze the basket with the ground herb (it should be a solid 'cake' on the inside of the basket,) and the heavy cutter/shedder plate. Plastic bag them so they don't pick up moisture. Freeze the solvent.

4) You can either pour the solvent through the plunger opening on the lid; or run it without the lid, and squirt solvent with a wash bottle.

The above post used hexane for the initial extraction and elution, why not use pentane, less smell, and a safer Class 3 rather than Class 2 food and drug solvent.


Should be good for a super cold ethanol quick wash? And then hit it again with room temp solvent for oral meds.

[SkyHighLer]

^^^ Another, wetted paper filter in the Acme 6001 basket, dump activated carbon (charcoal) powder through the plunger opening to form a thick packed filter, hit it with your oil solvent solution and out comes, near clear?? And with way less solvent/oil loss than a Buchner.

On that drift, line the basket with a one micron sock filter...

Or line the basket with a really 'tight' filter, and you can filter mold without the hassle of syringe filters.


I didn't see anyone using a centrifugal juicer as a DIY centrifuge at YouTube, maybe underground chemists are aware of the idea, has anyone run across it?

[SkyHighLer]

The bee keeper/bio diesel guys have a basic centrifuge design, see the video link below, and unless I'm missing something, you'd get the exact same action by blocking the Acme 6001's basket's filter screen with something, and pouring solvent/oil slowly down the plunger opening... the unit is designed to handle overflow, it will catch in the lid bulge, and flow down and out through the spout.

The Acme 6001 runs at 3,600 rpm, and if you use a Variac as mentioned in one my posts above, you can overdrive it by as I recall, about ten percent along with varying the speed.

https://youtu.be/PsLGX-RbKuQ

[SkyHighLer]

^ Found a Youtube video of how to do just what I described above to filter waste vegetable oil, the Omega 1000 is very similar to the Acme 6001,

https://youtu.be/rS26K9xt3Zg