Salvia Divinorum Extraction Tech: Isolation of Salvinorin crystals from black wax

About this extraction process

This extraction and refinement process is the easiest method with the highest extraction/processing efficiency I have found for obtaining high purity salvinorin which is accomplished through directly isolating salvinorin crystals contained in crude Salvia divinorum extract (AKA “black wax”). Aside from this extraction and processing method which I believe is probably the most yield-efficient, there are no other means I am aware of to obtain relatively high purity salvinorin other than through the use of partitioning and column chromatography or through using the somewhat inefficient process of doing multiple washes to crude extract with small amounts of solvents which salvinorin is weakly to strongly soluble causing greater losses with each additional cleaning of the extract. This tech will guide you through a new refinement process which directly isolates salvinorin crystals from crude extract using nothing more than common household solvents, utensils, mixing bowls and glasses which in the end, if great care is taken will net you an amount of high purity salvinorin crystals with minimal processing loss.


How it works

In this refinement process the salvinorin crystals which have formed within crude extract can be completely isolated. The process first separates most of the tannin impurities from the extraction solvent through natural settling of the tannin particles in the fluid which are then removed prior to evaporation. After complete evaporation of the extraction solvent, the still moist extract solids which remain are scraped up and placed in a small glass container and mixed with warm water to remove the remaining tannin impurities from the extract, discarding the water after each wash of the solids. Next, the solids are fully dried of all water moisture and then mixed with clean naphtha to wash the dark waxy impurities out of the extract, waiting for the crude salvinorin particles of extract to completely settle through the fluid to the bottom of the glass before pouring the fluid off after each wash. The naphtha washes to the extract are repeated over and over again until the solvent no longer continues to take on additional color. After most of the waxy green compounds have been removed from the exact solids by the naphtha washes the remaining solids are then mixed with a small amount of fresh naphtha again which is poured completely out (extract and naphtha together) into a small glass container which is then completely heat evaporated at approximately 125 degrees Fahrenheit. During heat evaporation of the naphtha a pronounced physical separation between the salvinorin crystals and the remaining waxy impurities occur which causes the salvinorin crystals contained in the extract to collect in the bottom of the evaporation bowl while at the same time forming a waxy crust of impurities on top which can then be peeled away to expose the crystals below.

The Process

Use high purity 99% Isopropanol (IPA) or 95-98 pure ethanol alcohol for this extraction method. 70% IPA has far too much water in it to be effective for extracting salvinorin off of the leaf in the short amount of time used and is not nearly as efficient at getting at all of the salvinorin like high percentage alcohols are. 99% IPA may be hard to find in some areas but can almost always be found if one is persistent enough searching for it. Acetone can be substituted for alcohol, see note three of this tech for more details.

Extracting the leaf and tannin removal

Extract dried finely crushed Salvia divinorum leaf three times over for at least five minutes each time with room temperature 99 percent isopropanol which must be at least 68 degrees F. or higher temperature. Pre-warming your container of alcohol/IPA to about 100 degrees F. via hot water bath is better than room temperature but is not required if you have extracted the leaf long enough (If using acetone see note three near the bottom). It is not necessary to powder the leaf prior to extraction as had been assumed in the past, recent findings by Daniel Siebert have determined that the salvinorin contained in Salvia leaf is actually deposited on the outside of the leaf rather than being contained in any relative concentration inside the leaf itself. When extracting the leaf each time through be sure to completely cover the leaf with enough solvent that you have at least an inch of fluid above the leaf and continue to mix the leaf the whole time while in the fluid. After removing all of the leaf particles let the combined solvent from all three extractions sit undisturbed in one container for at least 24 hours (in complete darkness) so that most of the micro-fine particles of tannin will settle to the bottom of the container, then leaving the sediments behind by very carefully pouring the precious fluid off of the tannin particles into another settling container to sit undisturbed for another 24 hours. After another settling you will probably find more tannin particles in the bottom of the container. Pour the fluid off into another clean container and let it set an additional 12 to 24 hours. When every bit of the tannin has settled out of the solvent it should be translucent, it will be light to dark colored green but should not have any amount of cloud to it or it still contains an appreciable amount of tannin.

Evaporation of the extraction solvent and further tannin removal using water

Once you have removed all of the tannin from the liquid you can through settling then let the Isopropanol completely evaporate in a wide glass Pyrex cooking pan, the wider the better so that you can have as large a surface area as possible to help speed evaporation. When evaporating the extraction solvent to obtain the extract solids it is extremely important that you make sure that all of the alcohol is completely evaporated but that the extract itself does NOT completely dry. Once the alcohol is gone you will find that in addition to the extract solids an amount of water will remain in the container which takes much longer to evaporate. Because the remaining water (often yellow colored) will contain large amounts of tannin be sure to pour all of it off of the solids, taking care not to let any of the small particles to go out with it. Do not allow the extract to dry because it must still be moist from the water for the next step to work. If the extract is accidentally allowed to completely dry the following water washes will not penetrate into the waxy material well enough to remove additional tannin. Next scrape every little bit of the wet extract off of the glass, even the dried films which you will find coating the upper sides of the container and add all of it to a glass container with between an ounce to a quarter cup of warm to the touch water (for extractions of 100 to 1000 grams of dried leaf) and crush all of the clumps of extract into as fine a consistency as you can by rolling the material between your fingers while in the water. After you have removed all of the clumps stir the extract into the water very vigorously for a minute and then let set for an hour or two or for however long the particles stirred up into the water take to settle out, perhaps many hours if using a cup or more of water at a time for each wash and how much leaf you have extracted. Once the salvinorin particles have settled to the bottom of the glass or jar of water slowly pour the water off of them, leaving all of the fine particles in the bottom. Now add another glass of water and do it all over again. Repeat until the water no longer takes on any color, usually a yellowish hue when you begin, to completely clear without color when you are done. The water used to remove additional tannin from the extract can be discarded once you are done with this step. Note: Since salvinorin won't dissolve into water this method will work to remove the remaining tannin without loss of salvinorin, if you wait long enough for it to all settle out.


Removing chlorophyll and waxy lipids from dried extract using naphtha

Upon completing several cycles of water washing the extract you will hopefully have removed all of the remaining tannin which is a major block to obtaining high purity salvinorin. Now completely dry the extract by spreading it out in a thin layer and placing in an oven set to 100-125 degrees F. for however long it takes to dry. Ambient temperature air drying will also work just fine but takes much longer, just to be safe against the possibility of UV light affecting the salvinorin put the extract in a dark place if drying it that way. It is ok to expose the solvents and salvinorin to normal room lighting while actively working the extraction as long as you are not in direct sunlight, but if at all possible avoid direct sunlight or UV light from florescent lighting, especially when wet with any kind of solvent.

Once the extract is completely dry try to crush it as finely as possible. Now mix the dried extract into 25 to 50 ml (close to an ounce or two) of pure room temperature naphtha and continue to work the extract into as fine a form as you can. Rolling the naphtha wetted extract between my fingers has worked best for me but crushing with a spoon while in the solvent will also help. Once all of the extract has been completely dissolved into the naphtha and has the consistency of extremely fine sand or better, pour all of the naphtha and extract together into a small but tall narrow glass container which can hold all of the extract and fluid in a vertical column only a few inches tall. Let the naphtha sit undisturbed for an hour or more. After awhile you will see that some very fine particles have dropped to the bottom of the glass, these particles are salvinorin crystals which will still have an amount of chlorophyll and waxy lipids mixed in with them. To be sure the majority of the super fine particles of salvinorin have dropped out of the naphtha you must wait until the fluid becomes translucent or clear enough to see through the glass which may be difficult if strongly colored by chlorophyll, but will become easier with each subsequent washing of the extract solids.

Once the fluid is no longer cloudy and you believe most of the particles have settled to the bottom then very slowly, without allowing any of the solids in the bottom to escape, pour all of the naphtha out of the glass leaving the fine solids behind. Set the solvent you have just poured off aside for 24 hours to get the last ten percent or more of the salvinorin which will continue to fall out of the fluid. Next take the glass you have just poured all of the naphtha out of while leaving the rather small amount of crude salvinorin solids in the bottom of the glass behind and add more Naphtha. Do it all over again and stir it up really well, just for a minute or so. As you do so the solvent should continue to take on a green color as long as there are more waxy lipids in the extract. Keep doing this step of adding naphtha, waiting for the salvinorin to settle and pouring the fluid off (saving the salvinorin particles in the same glass) over and over again until the fluid will no longer continue to take on much more color. Now, the extract should be well over fifty percent pure, perhaps as high as seventy five percent pure if you have done several naphtha washes. Before the next step pour every drop of naphtha off of the extract. Note: If a full cup or more of naphtha is used for each wash of the extract it may take hours for most of the particles to settle each time, the fluid can be colored but should not be at all cloudy or it still contains a large amount of ultra fine salvinorin particles. One quick way of checking to be sure all of the particles have settled is to take the glass of naphtha into a darkened area and shine a small flashlight through the top of the fluid. If the fine particles have not all settled yet you should then be able to better see them floating in the fluid. Don't worry about light interactions when doing that, you are only using a flashlight with very little UV output, if any.

Final processing to isolate the salvinorin crystals

In this next step add an ounce or so of clean naphtha to the extract and swirl it around in the fluid for a few seconds and then pour all of the naphtha along with all of the solids into a small four inch diameter (or smaller if having extracted from less than 100g of leaf) clear glass spice bowl and place the bowl in a box heated to somewhere between 100-125 degrees F. for heat evaporation. I believe higher temperatures will work just fine but you must not reach a temperature high enough to cause the naphtha to boil. For safety sake this should be done outside in a covered area using a small box which is somehow heated but which also allows plenty of air ventilation without using a light bulb or red hot heating elements. It is important that the bowl is not at all disturbed while evaporating completely down so you can't use a fan or allow air to disturb the surface of the bowl of naphtha, but at the same time be sure to allow the vapors to escape the box too. I have done this by placing a small spice bowl (no more than 1 ounce of naphtha in it) as far away from the heating elements as I could place it in a large electric oven with the door cracked open a couple of inches but WARNING... this is probably inviting a fire hazard or worse if just the right concentration of fumes hit the ovens red hot heating elements as it tries to regulate the temperature with the door cracked open. Once the Naphtha has completely evaporated and the extract is completely dry to the touch (after cooling) you will find that the bowl will have a thin green to black appearing paper-like skin on top which can be pealed away to expose a quantity of salvinorin crystals which should exceed 95% purity, if you have successfully removed all of the tannin impurities in the first steps of the process first. The salvinorin may or may not appear to be crystalline but when viewed under a microscope can clearly be seen to be small crystals and when shined under bright light will sparkle as you handle them.

Purity confirmation

If you have successfully removed all of the tannin from the extract and removed enough of the lipids and chlorophyll from the extract you will find nothing but loose crystals under the top waxy layer. However, unless viewed with a microscope you can't know for sure if you only have crystals or have a mix of crystals and fine tannin particles. If you are not convinced that the extract is fairly pure or just want to make sure you don't have any tannin in it, as a purity confirmation step, depending upon the amount of leaf extracted, dump all of the dried extract into room temperature acetone and thoroughly stir the solvent until completely dissolved. 100 ml of room temperature acetone should easily be able to dissolve all of the refined salvinorin extracted from as much as 1000 grams of average potency dried leaf, but if having extracted a full kilogram of leaf I would use at least 125 ml of acetone, just to be sure. Of course, use a proportionately larger volume of acetone for this step if having extracted from a larger amount of leaf. If the salvinorin is fairly pure and you have stirred the extract enough to completely dissolve every bit of it into the fluid when you are done the solvent should not have a cloudy appearance. As in earlier steps of the process (depending upon how much chlorophyll and lipids have been removed by the naphtha washes) the fluid can be a slightly yellow to dark green color but never cloudy. If you see any cloudiness of the acetone after having stirred the fluid for two or three minutes, the amount of time it usually takes to fully dissolve as much as 2 grams of high purity salvinorin into 100 ml of acetone, this is an indication of ultra-fine tannin contaminates being present in the fluid which after being stirred up into the acetone can take as many as two days to fully settle to the bottom again. If the fluid is completely translucent allowing you to see through it (as long as it isn’t too darkly colored by chlorophyll) you can then pour the acetone out into a dish for evaporation. At this point I like to evaporate the solvent into a small spice bowl and let it evaporate in a dark place over a period of days. Sometimes I come back to find wonderful little crystalline formations, others an uninteresting crust which although flat is actually completely crystalline when viewed under high magnification.

If after a good stirring and even going to the extent of warming the container of acetone to 120 degrees F. in a hot water bath and the fluid is still found to be cloudy then seal the container and let it sit in a dark place for 24 hours to wait for the contaminates to settle to the bottom of the glass. After settling carefully pour the acetone off of the sediments without allowing any to go out with the fluid as you are pouring the solvent into another container and let the fluid sit for another 12-24 hour period of time to see if more falls out, keep doing this over and over until all of the tannin sediments have stopped falling out of the acetone. After all of the tannin has been completely removed from the solvent you can then evaporate the fluid in a small glass dish which if done slowly enough will likely form into relatively large visible crystals, if not crystals then a very pure crust which because salvinorin sticks to glass so well will need be scraped off for collection with a knife. If the extract does not stick to the glass either as crystals or form a hard crust through and through which also sticks to glass the extract likely isn't very pure. The only exception to that general rule I know of is this particular extraction process where the salvinorin crystals are isolated directly out of the “black wax” (crude extract) without being dissolved again by solvent. Since this process removes most of the waxy compounds extracted from the leaf through the naphtha washes to the extract which will not dissolve salvinorin, and then through further processing produces a physical separation of the remaining waxy impurities from the salvinorin crystals they can be found to be laying completely loose in the bottom of the bowl, otherwise salvinorin sticks to glass when evaporated out of solvents which it is soluble to.

Note 1: Alcohol/IPA extractions. Extracting leaf with isopropanol or high proof ethanol warmed to at least 100 degrees F. will increase the solubility of alcohol to extract salvinorin from leaf more thoroughly and quicker than when at room temperature but I still recommend extracting the leaf for at least five minutes each time, three times over. If you are concerned you might be leaving salvinorin behind when using room temperature alcohol extract the leaf as many times as you wish for as long as desired but keep the leaf in the dark while in solvent for longer periods of time.

Note 2: Used naphtha. Once you are sure all of the salvinorin particles have settled out of the naphtha used to wash the extract by letting the fluid sit undisturbed in a glass container for at least 24 hours and have collected what ever additional amount of salvinorin particles have fallen out you can then discard the fluid because salvinorin is insoluble to it.

Note 3: Extracting with acetone. Some individuals believe the molecular ester rings of salvinorin can be easily hydrolyzed making the substance less potent if left in water for a period of time. Although I have not found this to be the case, if you are at all concerned that the extract might be weakened by water washes then extract the leaf with clean distilled reagent or technical grade acetone instead of 99% IPA or high proof ethanol and completely skip the water washes. When using acetone without the water washes called for in this tech extra care should be attended to assure that every bit of the tannin which can settle out of the extraction solvent falls out of the fluid before evaporating the solvent. Also, if you have solely chosen to use acetone in an effort to minimize the amount of water in the solvent the leaf should first be completely dried in an oven set to about 125 degrees because most dried leaf has close to 15 percent water moisture in it by weight, even if it feels dry to the touch. If the leaf isn't first oven dried prior to extraction this will result in a portion of the moisture in the leaf to be drawn into the Acetone along with an amount of tannin which is highly water soluble.

Due to the super solubility of salvinorin to room temperature acetone the leaf need only be extracted three times over for 3 minutes each time instead of the required five minutes I have specified for room temperature alcohols, discarding the leaf afterwards because you will have removed all but a minute amount of the salvinorin which coats the outside of the leaf in a very short time, almost all of it after the second extraction. Although there is a very small amount of salvinorin contained in the leaf itself most coats the outside of the leaf. Because of this the leaf could just as well be extracted in whole uncrushed form however this would require far more solvent than necessary to cover the leaf causing more work for you. If intending to extract with acetone you might consider chilling this solvent to near zero degrees F. and extracting the leaf three times over for three minutes each time (the same as at room temp.). Chilled acetone is wonderful for Salvia extractions because when cold will cause most of the chlorophyll and lipid contaminates to be left behind producing a much cleaner extract which is far easier to refine requiring fewer washes to the extract with naphtha. The solubility of salvinorin to acetone chilled to as low as -15 degrees F. is still several times higher than that of room temperature 99 percent IPA or 98 percent ethanol and because of this is an extremely good solvent for extracting Salvia whether the fluid is at room temperature or far below. If using chilled acetone upon evaporation the extract usually has so little waxy impurities that the salvinorin will form into pieces of high purity crystalline crust which when further processed by this method may not produce individual crystals but will isolate extremely high purity salvinorin particles which are every bit as potent. Sorry, if you are wondering if cold isopropanol or ethanol can be used to reduce the amount of contaminates extracted from leaf I have found that chilled alcohols are useless for efficiently extracting salvinorin, extracting only a small percentage from the leaf when cold and should only be used at normal room temperature or higher, about 20 degrees C. or at least 70 degrees F.

Once the acetone from either a room temperature or chilled extraction has completely evaporated scrape up all of the completely dried extract (no water moisture!) into a small 25 to 50 ml glass container for the naphtha washes. Be sure to get every bit of the extract off of the glass of the evaporation container, including all thin films which may have deposited on the sides because these crusty light green colored coatings are mostly high purity salvinorin which often deposits on the upper sides of the glass as the fluid level is reduced through evaporation. Continue processing the extraction the same as is shown for the 99% IPA extraction but be sure to do the final purity confirmation step of re-dissolving the cleaned extract into 100 ml of acetone (for extractions under 1000 grams of dried leaf) and then letting the container sit undisturbed for at least a 24 hour period of time, longer is better but be sure to keep the acetone in complete darkness the whole time while waiting and cover to prevent evaporation.

Note 4: Ester rings. I don't believe that the water washes of the extract will cause changes to the ester rings because the salvinorin which coats the outside of the leaf is regularly wetted by rain water as the plant grows (unless grown indoors and misting isn't done to the plant). I have had salvinorin tested by HPLC which had been boiled in water for several hours which didn't show problems with it at all, but that was only one individual testing one batch. Further testing would be needed to confirm those results but even then room temperature to warm water shouldn't be a problem to worry about, considering the leaf gets wet in it's normal environment anyway.

Note 5: Evaporation condensation. If evaporating the extraction solvent in a broad glass pan using a fan hurry things up by gently blowing across the surface of the fluid, whether having used isopropanol or acetone to extract the leaf you will find that due to rapid cooling an additional amount of water will condensate into the liquid which you can use to your advantage. Once all hint of solvent is gone from the fluid (smell it) and you are sure it is only water carefully pour it all off of the extract solids making sure that none of the fine green particles go out with it. The water found remaining in the evaporation container is usually a creamy yellow color which only contains large amounts of tannin.

Note 6: Ultraviolet sensitivity of salvinorin: Ultraviolet light has been reported to quickly destroy the potency of Salvinorin A, especially when in solvents or while on leaf wet with solvents. Common sources of UV light are direct sunlight and some kinds of florescent lighting. When extracting Salvia divinorum leaf do not do so in direct sunlight and minimize the amount of time the extraction solvents are exposed to direct light of any kind while containing salvinorin.

The following photographs are of salvinorin crystals obtained strait out of crude extract from a 99% IPA extraction.

The photograph on the left was taken on macro within about three inches of the bottom of a regular drinking glass used to evaporate naphtha cleaned extract that had about a half inch of clean naphtha stirred in just before placing the glass into an oven for evaporation. The smooth layer you see is a waxy crust of chlorophyll and lipid waxes which formed on top of the salvinorin crystals below it. I tore a portion of the wax off the top to show the crystals underneath. The second photograph was taken with a zoom stereoscope set to approx. 25X magnification, the third even further magnified and the last shows the same crystals with a dime which appear to be more golden than yellow due to different lighting.



WARNING:

No one should ever use Salvia divinorum or salvinorin in any form whether enhanced leaf or tincture without first having done enough research to know all of the possible effects produced by this substance, as with any intoxicating substance psychotropic or not. Also, individuals who have had serious psychological problems in the past or who are currently being treated for any kind of psychological problem should not use Salvia divinorum without first consulting their doctor. The best warning against the use of pure to crude salvinorin I have seen can be found at Daniel Siebert's web site at the following URL: http://www.sagewisdom.org/caution.html

Smoking the crystals or refined salvinorin has been reported to be extremely hit or miss and when it misses often leaving salvinorin residue in the pipe causing the next attempt to burn far too much material. Because of this possibility smoking salvinorin itself isn't something I would want to try, even if I have accurately measured the weight of the dose. However, there is another way a friend of mine came up with which is much safer and that is to dissolve the crystals into solvent and then evaporate it on something else you can smoke.

If you know the solubility of the solvent you are using to drip onto leaf (or what ever) then you can get close to a standardized method of dosing. For example, you can dissolve as much salvinorin as 99 percent isopropanol can hold and then use an eye dropper to slowly drip it onto cigarette papers. If you evenly spread the fluid across the whole paper and let it dry, depending upon how much fluid was evaporated on the paper you would know the approximate amount of salvinorin distributed on any given portion of it, as long as you are careful to avoid making hot spots where too much material cakes up in one spot.

Acetone would be ideal for this because it requires so much less solvent, just a few small drops onto paper ought to be enough if you have dissolved a known amount of salvinorin into a measured amount of acetone (completely dissolved with absolutely no solids observable, completely clear liquid). At room temperature acetone has been reported to be able to hold 23 mg of salvinorin per ml of fluid in the fully dissolved state where 99 percent isopropanol holds closer to a maximum of .75 mg per ml of fluid (less than 1 milligram per ml).

Through this method one is able to reliably burn a dose with so little smoke it is essentially the same as if having smoked the crystalline material itself. Of course, the papers would then need to be cut up into smaller pieces due to the amount of salvinorin which can be contained in one single piece.

If you would like to see over 100 pictures of salvinorin crystals join this group and go to the photo files: http://groups.yahoo.com/group/Salvinorin

[Edited on 28-12-2005 by Orb]

Very interesting, and nice extraction demonstration.
I suppose that this is the structure of the alkaloid


One major problem I can see is that those leaves aren't exactly widely available... unless seeds are OTC or something.


Please bear in that this is not a drug forum though.

Do you know how, in biochemical terms, this ocmpound works?

Yes, NJF, it is a kappa agonist, some brief info can be found here: http://www.erowid.org/plants/salvia/salvia_info5.shtml

+ much more by searching the web...

Click this photograph to see a large .98 MB photograph of the salvinorin crystals which were isolated using this process: