Register ICMag Forum Menu Features Search Today's Posts Mark Forums Read
You are viewing our:
in:
Forums > Talk About It! > Cannabis Concentrates > Preparation of crystalline THCA

Thread Title Search
Post Reply
Preparation of crystalline THCA Thread Tools Search this Thread
Old 11-15-2015, 11:18 PM #1
live resin
Member

Join Date: Apr 2015
Posts: 193
live resin will become famous soon enoughlive resin will become famous soon enough
Preparation of crystalline THCA

1. Extract fresh plant material with 0.1% acetic acid v/v in hexane. Filter and remove solvent by rotavap. The purpose of the acidified extraction solvent is to minimize ionization of the cannabinoid acid which would hinder subsequent purification steps

2. Pass the THCA rich solution through a column packed with Sephadex-LH20, eluting with 2:1 chloroform/dichloromethane. Collect the THCA-rich fraction.

3. Redissolve the crude THCA in methanol, filter insoluble material, remove solvent with rotavap

4. Redissolve crude THCA in pentane, filter, and rotavap to give THCA crystals

* All solvents and chromatography materials were obtained off the shelf from a local lab supply shop. 10L rotavap obtained from BHOgart
live resin is offline Quote


10 members found this post helpful.

Click to shop for Extractors and Hardware
Old 11-16-2015, 02:54 AM #2
live resin
Member

Join Date: Apr 2015
Posts: 193
live resin will become famous soon enoughlive resin will become famous soon enough
I know I'm not the first to see this patent for this and copy the procedure, has anyone else had success with this?
live resin is offline Quote


Old 11-16-2015, 06:21 AM #3
G.O. Joe
Member

G.O. Joe's Avatar

Join Date: Oct 2008
Location: Ditchweed City
Posts: 967
G.O. Joe is just really niceG.O. Joe is just really niceG.O. Joe is just really niceG.O. Joe is just really niceG.O. Joe is just really niceG.O. Joe is just really niceG.O. Joe is just really niceG.O. Joe is just really niceG.O. Joe is just really niceG.O. Joe is just really niceG.O. Joe is just really nice
Quote:
Originally Posted by live resin View Post
* All solvents and chromatography materials were obtained off the shelf from a local lab supply shop. 10L rotavap obtained from BHOgart
Quote:
Originally Posted by live resin View Post
I know I'm not the first to see this patent for this and copy the procedure, has anyone else had success with this?
What was your column loading ratio? What was the flow rate and how many column volumes of solvent were necessary to start and complete the elution of THCA, and how long did that take? How much did the Sephadex swell with that solvent and how much did it take to fill the column and how much did that cost? How is the Sephadex cleaned for reuse?

The patent, I do know is US 7,700,368. Those details are not in it.
__________________
In the clinical field, the practical application of these substances must be awaited with the usual necessary patience. - Roger Adams
Marihuana
February 19, 1942
G.O. Joe is offline Quote


4 members found this post helpful.
Old 11-17-2015, 03:39 AM #4
thegreenman91
Member

thegreenman91's Avatar

Join Date: Jan 2015
Posts: 167
thegreenman91 is on a distinguished road
What kinda yield using this method?

How many hours of work total?
thegreenman91 is offline Quote


Old 11-18-2015, 02:38 AM #5
G.O. Joe
Member

G.O. Joe's Avatar

Join Date: Oct 2008
Location: Ditchweed City
Posts: 967
G.O. Joe is just really niceG.O. Joe is just really niceG.O. Joe is just really niceG.O. Joe is just really niceG.O. Joe is just really niceG.O. Joe is just really niceG.O. Joe is just really niceG.O. Joe is just really niceG.O. Joe is just really niceG.O. Joe is just really niceG.O. Joe is just really nice
Is someone getting quotes on the sort of shiny new industrial gel chromatography system you guys would want? We won't tell.

The patent specified a column 1.5 meters tall filled to an unspecified height with 400 g. of the Sephadex, loaded with the dissolved extract of 100 grams of something. Let's say it was 20 grams of extract - 1:20 column loading is not bad at all. But, the LH-20 product instructions suggest a flow rate of 1-10 cm./hr. Compare this to the level of detail in El-Sohly's 6,730,519.

There are faster, dirtier, much, much cheaper methods that scale up well.
https://www.erowid.org/archive/rhodi...atography.html
__________________
In the clinical field, the practical application of these substances must be awaited with the usual necessary patience. - Roger Adams
Marihuana
February 19, 1942

Last edited by G.O. Joe; 11-18-2015 at 02:50 AM..
G.O. Joe is offline Quote


1 members found this post helpful.
Old 11-18-2015, 03:20 AM #6
oceangrownkush
Senior Member

oceangrownkush's Avatar

Join Date: Mar 2011
Posts: 1,375
oceangrownkush has much to be proud ofoceangrownkush has much to be proud ofoceangrownkush has much to be proud ofoceangrownkush has much to be proud ofoceangrownkush has much to be proud ofoceangrownkush has much to be proud ofoceangrownkush has much to be proud ofoceangrownkush has much to be proud ofoceangrownkush has much to be proud ofoceangrownkush has much to be proud ofoceangrownkush has much to be proud of
Would crystalline THC be snortable? I would love to rack up lines of Hash.
__________________
Quote:
Originally Posted by Cannavore
laws will eventually change. it can only get better. until then i won't acknowledge them anyways.
oceangrownkush is offline Quote


1 members found this post helpful.
Old 11-18-2015, 03:32 AM #7
Phineas Freak
Member

Phineas Freak's Avatar

Join Date: Apr 2015
Location: floating
Posts: 92
Phineas Freak will become famous soon enough
I guess THC can be taken up somehow by mucous membranes, analog to Sativex.

I wonder what the effect of eaten THCA is?
Has anybody tried? Is it psychoactive or not? Does it affect pain?
Phineas Freak is offline Quote


Old 11-18-2015, 03:51 AM #8
Avinash.miles
Caregiver Extraordinaire


Avinash.miles's Avatar

Join Date: Apr 2010
Posts: 7,527
Avinash.miles has a reputation beyond reputeAvinash.miles has a reputation beyond reputeAvinash.miles has a reputation beyond reputeAvinash.miles has a reputation beyond reputeAvinash.miles has a reputation beyond reputeAvinash.miles has a reputation beyond reputeAvinash.miles has a reputation beyond reputeAvinash.miles has a reputation beyond reputeAvinash.miles has a reputation beyond reputeAvinash.miles has a reputation beyond reputeAvinash.miles has a reputation beyond repute
Avinash.miles is online now Quote


1 members found this post helpful.
Old 12-02-2015, 03:32 AM #9
live resin
Member

Join Date: Apr 2015
Posts: 193
live resin will become famous soon enoughlive resin will become famous soon enough
12k for the factory refurbished chromatography system. The 10L rotavap was 8k
live resin is offline Quote


2 members found this post helpful.
Old 12-02-2015, 05:32 AM #10
oceangrownkush
Senior Member

oceangrownkush's Avatar

Join Date: Mar 2011
Posts: 1,375
oceangrownkush has much to be proud ofoceangrownkush has much to be proud ofoceangrownkush has much to be proud ofoceangrownkush has much to be proud ofoceangrownkush has much to be proud ofoceangrownkush has much to be proud ofoceangrownkush has much to be proud ofoceangrownkush has much to be proud ofoceangrownkush has much to be proud ofoceangrownkush has much to be proud ofoceangrownkush has much to be proud of
Couldn't you just purge it like BHO? I know people use Hexane to make extracts and don't spend 12k on their desiccation chamber. Has to be an alternative to the rotovap.
__________________
Quote:
Originally Posted by Cannavore
laws will eventually change. it can only get better. until then i won't acknowledge them anyways.
oceangrownkush is offline Quote


Post Reply

Thread Tools Search this Thread
Search this Thread:

Advanced Search

Posting Rules
You may not post new threads
You may not post replies
You may not post attachments
You may not edit your posts

BB code is On
Smilies are On
[IMG] code is On
HTML code is Off


All times are GMT +2. The time now is 09:12 PM.


Buy Cannabis Seeds at Seed Boutique


This site is for educational and entertainment purposes only.
You must be of legal age to view ICmag and participate here.
All postings are the responsibility of their authors.
Powered by: vBulletin Copyright ©2000 - 2017, Jelsoft Enterprises Ltd.