making salvia divindorum extract questions

[trav]

This is gonna be my first time making the extract and I read the coffeeshop way of doing it but isnt acetone and naptha pretty dangerous to use in a material you are going to be smoking once you add it to the leave?  I was thinking everclear may work because it can dehydrate also but like i said this is my first time and i dont know shit but i really dont want to die of poison or blow up my house so if anyone has a way for everclear or just any suggestions about the everclear and the toxicity of it please let me know before i make a batch

[nyko]

I know synch used naptha in his extraction and me and my friend had a good time with it, and didn't die :/

I'd wait to talk to someone who has extracted before though if i was you.

[Synchronium]

The only time using acetone/naptha/isopropanol is dangerous is when the product is smoked without allowing your extract time to dry.

If your extract smells even slightly chemical then it's not ready to smoke.

Also be careful with evaporating any solvents like that with heat as they're flammable. Use a hair drier but only in small bursts.

What exactly is everclear? Rubbing alcohol?

[trav]

Everclear is a grain alcohol can be 190 proof its a solvent i believe.  Many of the US provinces have made it illegal to buy Everclear and it's very uncommon to see the most potent of the Everclear products sold outside of America.

But how long would it take to dry the extract you make without any heat and just letting it sit or with just a hairdryer in small bursts.  A batch of 100g that is.

[Synchronium]

Well, Everclear would be just as dangerous to smoke as propanone/propan-2-ol/nathpha.

And it tends to take forever to dry. You have to remember to keep it in the dark, don't sit it in the sun. With a hairdrier on short busts, you could probably evaporate a batch in about 10 hours, then do the nathpha washes to purify the salvinorin-a (unless you're making 10x exract or lower). You then have to redisolve in as much solvent (maybe a tiny bit less) than you originally used and let that evaporate over your leaves, which will take a further 10 hours or so.

Quite a pain in the arse really.

Also, moved to salvia forum.

[trav]

ya seems like a pain in the ass really lol.  Think ill just stick to buying it until the summer time comes where i can do all that stuff outside and not in the house.  But i think i got the basics of making it though...i think ha

[nagual]

The guide at http://www.coffeesh0p.com/Info/Making_Salvia_Divinorum_Extract/ is lacking. 

Using any solvent other than acetone (i.e. propanone) is inefficient and you are throwing cash down the drain. Salvinorin A is several times more soluble in acetone than alcohols (methanol, ethanol, propanol, whatever).  If you use acetone, then a five minute initial wash is more than long enough to extract the Salvinorin A as it is very soluble in acetone.  Any longer than that and you'll extract all the sticky wax as well.  If you grind the leaf you'll just get more wax. 

Salivinorin A -> very soluble in acetone.
Wax -> not so soluble.

I'd like to re-emphasise the point about keeping the acetone/Salvinorin solution in the dark and keeping it cool.  Salvinorin A doesn't much like being in acetone and especially dislikes UV light when in solution.  I wasted my first batch by leaving it in a sunny window to evaporate.  I get better yield by leaving the solution in a dark cupboard and being patient. 

DO NOT USE A HAIR DRIER.  You should treat a bowl of acetone like a bowl of heated petrol. Pure acetone is more volatile than petrol and loves giving out all of its energy in one go when placed in a room with a heating element and air.  Believe the Guinness ads.  Respect the eyebrows.

[Synchronium]

Do you have any sources for that information?

I agree, the hairdryer method is a bit sketchy, but I've always found propan-2-ol to be quite reliable. It's slower & less efficient, but that means you  use a lot more of it, resulting in less losses. The extra wax procurred can also be extracted quite reliably with nathpha.

I'd say at this point, propanone would be the best choice to redisolve the salvinorin-a, as you need a lot less to disolve it all.

Points noted, and I'll probably edit the article at some stage after everything else already on my to do list.

But some reliable sources would be sexy.

[nagual]

I can do references.  It helps having access to computers in a university for them. 

I don't know what these guys intend to do with their 10g of pure Salvinorin A but I hope they don't waste it.  This quote comes from:
David Y. W. Lee, et. al., "New neoclerodane diterpenoids isolated from the leaves of Salvia divinorum and their binding affinities for human j opioid receptors", Bioorganic & Medicinal Chemistry 13 (2005) 5635–5639

"The dried leaves (4.6 kg) of S. divinorum were sequentially
extracted with hexane, acetone, and methanol.
The acetone extract showed the most potent binding
activity to human KOR [a.k.a. the Salvinorin A] ; the
hexane and methanol fractions were much less potent.
Following published procedures, the pigments in acetone extract were removed
by chromatography on activated carbon. Upon further
recrystallization from acetone and methanol, a significant
amount of salvinorin A (<10 g) was isolated. The
supernatant of the acetone extract was chromatographed
on a silica gel column and eluted with chloroform–
acetone to give five fractions. The fraction eluted
with chloroform–acetone (20:1) had the most potent
binding activity and was subjected to repeated silica
gel column chromatography to give three new diterpenoids:
divinatorin D (1), divinatorin E (2), and salvinorin
G (3), and 10 known compounds, divinatorin C (4),
hardwickiic acid (5), salvinorin-A (6), -B (7), -C (, -D
(9), -E (10), and -F (11), presqualene alcohol (12), and
(E)-phytol (13). The known compounds were identified
by comparison with their published data.21,23–26"

The following quote was taken from:
Thomas A. Munro and Mark A. Rizzacasa*, "Salvinorins D-F, New Neoclerodane Diterpenoids from Salvia divinorum, and an Improved Method for the Isolation of Salvinorin A, J. Nat. Prod. 2003, 66, 703-705

It suggests that acetone is good for extraction but is best when cooled. At room temperature, acetone also extracts lots of lipids (waxes and gunk).  It also says that methanol was used to recrystallize the Salvinorin A meaning that it is not very soluble in methanol.  It sounds like they were only learning to do the extraction for the first time so hadn't really perfected their method:

"During the development of an improved procedure for
the isolation of 1 [Salvinorin A] and 3 [C] from S. divinorum, three new
compounds were isolated: salvinorins D, E, and F (4-6).
Using several solvents, Gruber demonstrated that extraction
at room temperature gives a higher recovery than the
refluxing solvent used in the original procedures.  His
results suggest that 1 [Salvinorin A] decomposes rapidly in hot solution.
We found that extraction at room temperature in acetone
gave an excellent recovery. However, the pigments present
in the crude extract proved troublesome; the green-black
color made it almost impossible to distinguish the phases
during the solvent partitioning procedure employed by
Valdes and co-workers. Some coloration persisted even
after chromatography and recrystallization, as noted previously,
12 and the numerous pigment spots greatly complicated
TLC analysis. We therefore decided to decolorize the
crude extract by chromatography on activated carbon.13
This gave an amber terpenoid mixture from which pure 1
was isolated by recrystallization from methanol (giving a
total yield of 3.4 g/kg)."

The best "recipe" articles can be found at:
http://photos.imageevent.com/sphere/salviadivinorumextractiontech/Salvia%20divinorum%20extraction%20FAQ.pdf
http://photos.imageevent.com/sphere/salviadivinorumextractiontech/Chilled_acetone_extraction.pdf
http://ethnobotany.yage.net/salviax.html