Extraction of Sassafras ???

DjTime · Chemical Dj

never mind

joe_aldehyde · huxleys associate

i personally haven't steam distilled it, but still...you're gonna raise at least some suspicion if you're gonna buy that much root bark. the rhodium archive has some info on oil content of sassy root bark. UTFSE Smile

icecool · Insistent Chemist

Is it possible to distill sassafras oil in a rotavapor under vacuum.
Since distilling off solvents under vacuum goes very quick because of the rotating flask.
So I thought if you would use a rotavap for sassafras oil you can distill that very quickly.
Of course you would need to use an oil bath then.

primathon · modified

I don't have anything to back this with right now, but I remember asking Rhodium about this. He told me that using a rotovap will work very quickly, but at the tradeoff of purity. The slower you do it, the purer your fractions will be, especially under vacuum. I'm not sure exactly how this would apply to steam distillation, but you may want to look into it.

icecool · Insistent Chemist

No I just meant rotavapping it without water.
And with vacuum...
So no steam distillation, anyone else info about this?

DjTime · Chemical Dj

Why couldnt one boil the sassafras bark for hours then distill the whole liquid lot? Wouldnt the oils come out of the bark anyways and become part of the water solution?

icecool · Insistent Chemist

Well you could do that, but you will get quite a mess with that bark.
And do you know how much bark you would need to even get the tiniest amount of safrole.
You would need to buy kilo's and kilo's of that stuff...

MargaretThatcher · Sun Jun 19, 2005 4:58 am

I think steam 'distillation' is likely more efficient than boiling bark and distilling. Steam 'distillation' is a gas phase extraction: water vapour is passed through the bark at > 100 C bringing with it safrole vapour. If I were going to try a root bark extraction, I would build a steam extraction rig - that is how the industry does it and there must be some reason for that.

6o0538411 · Sun Jun 19, 2005 5:50 pm

Has anyone had experience with "Cinnamonium Camphora"... This stuff is all over where SWIM lives and is meant to be a rich source of camphor for which up to 80% of the brown camphor is sasaffras oil...

SWIM just wonders how you would go about extracting this from the plant material. They grow wild so much around here and there are trees of all sizes from seedlings to fully matured trees? What would be SWIMs best bet u think?

Star-light · Blacklight bulb

There are many varieties of Cinnamonum Camphora, some of which contain reasonable amounts of safrole, others do not. Even those that do require quite a bit of work to get the safrole out in a pure form.

The three varieties of Camphor Oils could be
distinguished as follows:

Formosan Camphor Oils = camphor-linalool
type and camphor-safrole type.

Japanese Camphor Oil = camphor-safrole
type.

Chinese Camphor Oil = cineole-terpineol-camphor

In Formosa, the camphor-safrole type as well as the Camphor-linalool type are produced, the former being the largest in quantity.

The essential essential oil that you are interested in is produced by steam distillation from the wood, rootstumps, and branches of the variety of Cinnamomum Camphora known as Hon-She, growing in Formosa and Japan. Along with the crude oil comes a solid, partly crystalline mass of crude Camphor. The oil is separated from the crude camphor by filterpressing. This yields the Crude Camphor Oil.

The crude oil is subsequently rectified under vacuum, and yields 50% of crude camphor. The remaining 50% of the filterpressed crude camphor oil is now free of camphor. It contains light terpenes, cineole, safrole, terpineol, sesquiterpenes and sesquiterpene alcohols. This is obviously the fraction you are interested in. These materials are then further separated in various fractions known as:

White Camphor Oil, the light fraction, contains Cineole and monoterpenes;

Brown Camphor Oil, the medium-heavy fraction which contains up to 80% Safrole, and some terpineol;

Blue Camphor Oil, the heavy fraction which contains sesquiterpenes

The white and the brown camphor oils both amount to about 20% of the crude total distillate from the wood, or each about 40% of the filterpressed, camphor-free oil.

As you can see, even if you have the right variety of tree, you are going to get less than 16% of safrole in the oil that you steam distill from the wood. In addition, you will have to distill many kilos of wood to get a kilo of oil.

To me it sounds like a lot of hard work that would be best utilised doing something else.

6o0538411 · Mon Jun 20, 2005 4:53 am

methyl_ethyl · Riedel De Haen

Do you think rather than using water as the solvent (aka steam) that maybe methanol or ethanol etc could be employed and improve extraction?

Continuous Soxhlet Extraction is being investigated by some industrious bees. Although the Soxhlets are scaled up for use with kilo's of plant material. In fact I think someone on this board has posted pictures of the soxhlet type apparatus that was constructed from OTC materials.

I think the extraction, which ever way you choose would be a breeze as compared to having to dig up the kilos of sasafrass roots, then stripping the bark from the roots. Harvesting the root bark fresh is an absolute must in regards to yield, as this is a volatile essential oil. Some people grind the bark into a slurry before extraction, I assume to expose more surface area to the solvent, or to reduce the displacement of the plant material in the "thimble" or extraction chamber for the scaled up soxhlet.

Obviously the main advantage of continous extraction would be that you have a much smaller volume of solvent extract to distill as compared to litres and litres of aqueous extract to distill / extract post steam distillation.

For any of those attempting steam distillation or continuous extraction please post your findings / experiences.

Regarding the Rotovap idea: I have always wondered about this. In fact I have a bunch of Sasafrass Bark in my freezer that I wanted to try to lyophilize and trap the volatiles in a 4L cold trap. I have a multi-port benchtop lyophilizer that I could easily pack a few kilos of pulverized root bark into ~6 of the ports. It's just a dream but I thought about doing a few runs. One with fresh rootbark, One with rootbark exposed to -80C before lyophilization, and just for shits and giggles I was going to immerse some of the bark into liquid N2 before lyophilization, to see if sublimation of the oil out of the bark was possible under high vacuum.

I have no reasoning behind my wanting to do this, it was just something that I wondered about and wanted to see if it was possible.

Maybe in my spare time...

regards,

m_e

riggie · Fri Jun 24, 2005 6:12 am

Hm, with mdma prices around 2500 euros now, not worth the trouble I belive

methyl_ethyl · Riedel De Haen

The price of MDMA has nothing to do with this thread

GOD · Tue Jun 28, 2005 3:53 am

swim did a soxhlet extraction a few years back, on local, dug up, fresh sassafras rootbark, around falltime IF he remembers correctly (thats when safrole content is supposivly highest).

he has absolutly no recollection of quantities used etc, but he seems to think a sohxlet fit for a 5L fb flask was used,......cant remember the solvent used either, but it was what was suggested by some bee's in the know.

he remembers thinking to himself "holyshit! hope swim never has to rely on this as a source, because its ALOT of work for such little product".

The extract came out bright red, and needed vacuum distillation, and he heard that it was eventually put to good use Wink

.

Maybe a search of the archives may produce a post or two- swims certain he would have reported.

Lots of work! He remebers thinking that he would probably hunt down directions for homemade stills made out of old milk cannisters/beer kegs (that used to be somewhere on the hive/net) and get a couple of them going in place of the 5L sohxlet he had at the time......

but then again, its been a few years, and swiG's memory is horrendous!