Salvia Divinorum Extraction and Refinement Tek. 9.9.6 (slow to load due pics)
Posted 02 April 2005 - 07:45 AM
The easiest and most efficient way I have found to get down to high purity crystalline salvinorin is very simple. I don't know if this works the same way when using Acetone to extract leaf, but this has worked every time for me when extracting leaf with 99% Isopropanol.
The following method can be used to obtain salvinorin crystals by extracting Salvia Divinorum leaf using 99% Isopropanol, removing all of the bits of leaf and then either filtering the extraction fluid or waiting for tannin sediments to fall out of the liquid to remove as much as you can that way first. Next, dissolve all of the extract into the Naphtha by hand working all of the clumps of extract into the Naphtha with a spoon until only fine granules remain in the fluid, then continuing to wash the extract several times over with more fresh Naphtha until it is obvious that the fluid has become ineffective for removing additional fats and Chlorophyll because the extract won't get much lighter with each additional wash, and the Naphtha has become a very light green translucent color. Each time you wash your extract with Naphtha the fine salvinorin crystals will be churned up into the fluid and take a half hour or more to settle to the bottom of the container, so be sure to set the glass your using for the Naphtha washes aside for at least 30 minutes between washings of the extract before pouring the fluid off the solvents. When you first start washing the extract with Naphtha the fluid will take on such a dark color that you will likely be unable to see where the fluid ends and the dark colored extract in the bottom begins. If after a half hour or more you are unable to see that the particles in the fluid have completely settled you can remove half of the fluid (as long as the glass wasn't filled more than 1/3 full of extract when it was dry) from the top using an eye dropper and then add more clean Naphtha to the glass stirring the extract for five minutes and waiting another 30 or more minutes for the fine salvinorin particles to settle again. After the second 30 ml wash of extract with Naphtha I have always been able to see a separation between the darker fluid and the lighter colored solid in the bottom of the glass. The amount of Naphtha used for each wash to remove Chlorophyll from the extract isn't critical, what ever amount is needed, you can use larger amounts without fear of loosing any of you salvinorin as long as you wait long enough for the salvinorin to settle to the bottom of the container each time. You can add four or more ounces of Naphtha at a time using a pint sized jar when cleaning your extract instead of a small shot glass and that will work out just fine, just keep adding and pouring off Naphtha until the extract is as clean as you can get it and then pour every last drop of Naphtha off of the extract and dry the extract until no hint of Naphtha remains. Collect all of the Naphtha used to remove lipid waxes and Chlorophyll together in one container and set it aside for several hours and check it to see if more salvinorin particles have settle out of the fluid. I have been able to find as much as 10% of the salvinorin in the bottom of the Naphtha that didn't settle all of the way out with each 30 minute settling, so never throw it away until you have checked hours later to make sure you are not wasting any of the salvinorin that way.
After your completely finished with the Naphtha washes and the extract is completely dry without any hint of Naphtha smell remaining, crush and mix all of the extract together in a bowl with a spoon as finely as you can so that it is completely powdered and then start washing the powder with room temperature water until it will no longer take on a yellow or brown color. This step is to remove additional tannin that might still be in the extract, I can usually remove the remaining tannin with just a few one ounce washes with water but you can use a full cup or more at a time of you wish as salvinorin is insoluble to water, but when using that much water at a time to clean the extract from a 100g or less extraction of leaf you might not see any color to the water because the small amount of tannin would be so dilute that it might not turn the water a darker color when using that much at one time, that is why I like water washing the extract in a small vial or shot glass so I can see for myself if much tannin came over. Once you can see that the water will no longer take on any color completely dry the extract of all moisture and then put all of the extract into a small shot glass or spice bowl at or under two inch diameter and pour in enough fresh Naphtha so that the extract has about a half inch of Naphtha on top, about an ounce is all you need. Thoroughly stir the extract into the solvent with a spoon and then place the bowl in an electric oven set to about 120 degrees F. with its door cracked open. Keep the glass of Naphtha as far away from the heating elements as possible because there is potential for fire. When using this technique by leaving the glass or bowl undisturbed while the Naphtha evaporates off the heavier salvinorin crystals will all settle to the bottom of the glass while the was forms an upper crust. Once completely dry place the glass container in a freezer for long enough to cause the top layer of wax to stiffen up enough to be able to peel off the upper crust by hand leaving almost pure golden colored to light green high purity micro-size crystals in the bottom of the glass. They might not seem like crystals unless seen under enough magnification, but they are.
Where can I get clean Naphtha?
I would never recommend using Naphtha for to remove the waxy lipid fats and Chlorophyll from Salvia extract to make commercial products to be sold to the public, but if you are just making it for yourself and follow up the Naphtha washes one last wash with 99% IPA or high proof drinking Alcohol you will wash out the majority of not all of the impurities which might have been introduced by the Naphtha.
It can be difficult to find Naphtha that will evaporate completely clean. Do not try to use any kind of Naphtha unless you are sure that it is only Naphtha and does not have oils, or rust inhibitors added to it, such as is common with camp stove fuels. What ever Naphtha that you choose to use completely evaporating at least one ounce or more of the batch of solvent you intend to use to see if any residue remains. A good check of hardware or store bought solvents is to evaporate out as much as you intend on using, but since your pouring the Naphtha off of your extract evaporating an ounce ought to be enough to see because you will have far less than that amount in your extract, once poured off. If you do not want to use Naphtha, you can use 98% Ethanol or 99% Isopropanol to clean the waxes out of an extract if you are very careful to use as little as possible you won't loose too much salvinorin, especially if the IPA is chilled, it will carry away even less salvinorin with each wash when chilled to 40-50 degrees F. because it is unable to hold as much salvinorin when cold but will still wash the waxes out. This might sound contradictory considering chilled solvents are used to help leave wax behind when extracting from leaf, but once it is extracted into a high concentration small amounts of cold 99 percent Isopropanol will remove some of the waxes with each wash, even when cold although marginal compared to room temperature Isopropanol it is one alternative to using Naphtha or room temperature Isopropanol which will work too but carries away more Salvinorin with each wash so use it sparingly. I have tried one brand of Naphtha lighter fluid sold under the brand name of Ronsonol and have been able to evaporate eight ounces of it completely out without a hint of residues, but some people object to using it because it contains less than 30 parts per million benzene. Considering that it is only used to clean the extract of the dark and waxy compounds and is not evaporated down into the extract itself and that benzene evaporates out very easily, I don't see it as a big issue but you should be aware of it. The amount of benzene that we each are exposed to on a daily basis (if you live in a city) is somewhere around 250 micrograms just from breathing the air and nothing more. The amount remaining from using Ronsonol lighter fluid to clean the wax out of extract will be far less than that, if you don't evaporate it down into your extract and just pour it off, probably a few micrograms.
Can I use any kind of 151 Proof Alcohol to make tincture?
151 Proof drinking Alcohol will work for home made tincture, it won’t be as strong as a tincture made out of 191 Proof Alcohol because it contains close to 25% water but it will work well enough. I have made tincture using 151 Proof Everclear so that there is no other taste added but others have reported using 151 proof rum which turned out to be very good. Tinctures made with 151 proof won't hold as much salvinorin because of the water but seem to work fine anyway, you just have to use more tincture for the same effect as commercially made tinctures that use 95-98% Ethanol.
Posted 02 April 2005 - 07:47 AM
As far as I know, no one is making a tincture that is strong enough to have effects with only a drop or two because salvinorin isn't very soluble in Alcohol, because of this you can't get enough salvinorin in the Alcohol to make it that strong. I have heard of using small amounts of Acetone which can hold more than 20 mg of salvinorin per ml of fluid and sublingually dosing with it as a tincture requiring less than 10% the amount of fluid required when using high proof Ethanol alcohol, but Acetone isn't something people normally want to put in their mouth and how toxic small amounts of Acetone might be if used sublingually as a tincture is something I have never looked into. Daniel Siebert's tincture has been tested by someone who says that they found it to contain 1.36 mg of salvinorin per ml of 98% Ethanol. I am not sure what the upward room temperature limit is, but I believe it to be somewhere around 1.5 mg per ml for 98% Ethanol, perhaps higher if some of the dark Chlorophyll compounds from the leaf are in it. It has been reported to me that when waxy lipid compounds from the leaf present in Isopropanol or high proof 98% Ethanol that it can hold larger amounts of Salvinorin per ml, but I have not been able to confirm this report yet. Also, I am not sure how much Salvinorin 151 proof Alcohol will hold on an ml basis with close to 25% water in it, probably around one mg per ml of fluid.
If extracting leaf with an average potency of 2.5 mg of salvinorin per gram of dried weight 100 gram of dried leaf ought to have at least 250 mg of salvinorin but due to extraction losses I wouldn't bet on being able to extract out more than 200 mg, especially if using 99% IPA which isn't as efficient as Acetone. If you extracted the leaf using 70% Isopropanol, even if for several days, it could be closer to 175 mg because the water in 70% isn't as effective making a solvent which is already weakly soluble to salvinorin even worse. An ounce of Alcohol contains 28 ml of fluid so if you extracted from 100g of average leaf using either 99% IPA or Acetone you ought to be able to make at least 4 to 5 ounces of strong tincture, depending on how much salvinorin is in your leaf and how efficiently the extraction went. I am being very conservative with those estimates, if your extraction went extremely well you could make at 6 ounces of tincture out of 100 gram of average potency leaf.
I tried to make Salvia divinorum tincture out of pure white crystalline salvinorin trying to dissolve 40 mg of white powder into 28 ml of 151 proof Everclear Alcohol by warming the Alcohol to near boiling and stirring it all it. Initially all of the salvinorin completely dissolved into the fluid, but as it cooled at least a quarter of the salvinorin crystallized back out of the fluid making it very clear that 151 proof won't hold what Daniel's 98% proof Ethanol can hold. Later I tried using the tincture and found it to be very weak without much if any effect. Then I made another batch of tincture with enough of the Chlorophyll compounds from the leaf to color the Alcohol a very dark green color and found that the tincture was then effective again. From this I gather that there must be something in the leaf which either helps sublingual absorption of salvinorin or somehow increases the amount of salvinorin that can dissolve into the 151 proof Ethanol. Perhaps both are true, these compounds allow Alcohol to hold more salvinorin and at the same time help with sublingual absorption? Maybe the green compounds from the leaf are not needed as much for a tincture made from super high proof Ethanol such as 98% Alcohol, I wish I knew the answer to this but I am unable to locally obtain that high of a proof of Ethanol to know. What ever the reason, if you are making a simple Salvia divinorum tincture with 151 Proof Ethanol you want some of the dark impurities from the leaf in it, they might even help make higher proof tinctures more effective too.
If want to make a 151 proof tincture that isn't as strong or harsh tasting as one made with all of the dark compounds extracted from the leaf you can improve the taste by removing a portion of these dark waxy compounds by washing the dried extract with Naphtha until it will no longer take on much more green becoming a light green translucent fluid, at that point stop washing the extract with Naphtha and pour off every last drop and completely dry the extract until no hint of Naphtha remains and reconstitute with Ethanol drinking Alcohol of your choice. If after removing as much of the dark Chlorophyll as you can with Naphtha and you continue to wash the extract with small amounts of 99% IPA as is done to clean the extract to a white purity at some point will take too much of the green compounds out and result in a weakly effective tincture.
Be sure to remove most of the tannin from the extract to be used for making tincture otherwise it will end up as brown sediment in the bottom of your bottle. Tannin is an acidic astringent, because of this I am wondering if small amounts of it dissolved into the water component of an Alcohol tincture might somehow help the absorption of salvinorin tincture because I have heard that small amounts of ascorbic acid (vit. c) and Menthol mixed into a high proof Alcohol also help absorption. If an acidic component helps bring blood to the surface of your sublingual membranes perhaps that's the reason why and the natural tannin in the leaf might also produce this same effect from its acidity.
Tincture burns my mouth very badly and causes a lot of pain every time I try to use it, is there a way of making a tincture that burns less?
If you dilute salvinorin tincture with small amounts of water it will burn less but also be proportionally less effective. One kind of salvinorin tincture I have heard about uses a mixture of 50% 151 proof Ethanol and 50% DMSO (70% pure) that has been reported by others to burn far less than tinctures made with 98% Ethanol. DMSO has been used for a long time in various tinctures, so this isn't completely new, although I have only heard of this being done for home made salvinorin tincture and not currently being sold as a commercial product. I have not worked with tincture using DMSO very much but I can offer the following: I purchased some 70% DMSO (30% water) at a local health food store and made a mixture of half DMSO to half Ethanol and found that it burned far less than tincture made out of 151 proof Ethanol alone, although I only tried one dropper load of it because I didn't like the idea of using DMSO sublingually so being unwilling to use enough of it I can't confirm whether it is an effective method or not. Perhaps an Ethanol/DMSO tincture burns less is due to the DMSO I used was close to one third water further diluting the Ethanol, or perhaps it was because small amounts of DMSO when used sublingually burn less than Alcohol does.
If making a tincture of out a mixture of Ethanol and DMSO the best way I can think to do it is to dissolve as much salvinorin as you can into hot DMSO until it will hold no more first, and then dissolve the remainder of the salvinorin into the Ethanol before mixing them together. I found that salvinorin will dissolve into heated DMSO but it doesn't appear to hold salvinorin as well as Ethanol, whether this is due to the solubility of salvinorin to DMSO itself, or the fact that the only DMSO I could find contained 30% water I don't know. As a side note I have tried dissolving large amounts of salvinorin into 70% DMSO and then tried to dose with it by rubbing it into the side of my arm but it had no effect at all except for making my arm red and stinging like hell. Apparently salvinorin is too large a molecule to be absorbed through the skin through the use of DMSO, or perhaps DMSO won't dissolve salvinorin finely enough to allow it to pass through the skin. One thing to consider about DMSO is that if you don't completely clean your skin first or have any contaminates in the fluid this solvent can induce contaminates right through your skin into your body which isn't a very good thing to do. Skin is meant as a protective barrier so using DMSO this way whether on your arm or sublingually might not be the best idea unless completely free of contaminates or materials which shouldn't be absorbed that way.
Posted 02 April 2005 - 07:48 AM
When I first started extracting Salvia divinorum leaf there wasn’t anything to be found on the net about extracting this leaf other than a brief mention on Daniel Siebert’s web site that isolating salvinorin required the use of an organic laboratory with a small mention of using separatory funnel. With that lead I was able to find that a mixture of aqueous Methanol (20% water mixed into it) and Hexane could be used to refine the waxy extract from an Acetone extraction of Salvia divinorum leaf. Searching the net I was able to find that by dissolving all of “black wax” extract into Methanol and then adding an amount of water to it to keep it from being able to mix with Hexane that by placing the Menthol together with Hexane in a glass container and vigorously shaking that the waxy compounds from the leaf would be transferred into the Hexane leaving most of the salvinorin in the Methanol solvent (I used Naphtha instead because it had nearly the same properties has Hexane.)
After waiting a few minutes the two fluids would separate into two distinct layers. That’s easy! I was able to remove most of the lipid fats or wax from the extract this way but try as I may, I was having difficulty with the extractions because I would always end up with far more green extract than possible. The leaf I was extracting produced close to two grams of green extract per 100 grams of leaf which should only produce about a quarter of one gram, or 250 milligrams of salvinorin when extracting average potency leaf. It took me a long time to figure out what was going wrong and that turned out to be tannin… most of the extract had loads of tannin in it! I found this to be the case by leaving the solvent from an extraction in a large bowl over night, waiting for the next day to evaporate it, the bottom of the bowl was covered with a very fine brown colored sediment which I thought could only be tannin from the leaf because it would not dissolve into solvents but would dissolve into water. From there, I found the biggest block to obtaining high purity salvinorin. I could then use a separatory funnel to refine the extract into a very high purity but using a glass funnel was a pain. I decided to try to use strait Naphtha on the extract to see how that might work out. Turns out, it worked great and from that point on I never used a separatory funnel again.
I found a way to extract, remove tannin and refine salvinorin into a white purity using nothing but a shot glass and two solvents, actually, only one is needed if you use Isopropanol to both extract the leaf and remove fats, but without using Naphtha to remove the lipid waxes prior to using IPA has higher losses. Even after finding out about the tannin impurities in the extraction fluid which were almost invisible I was still stumped from time to time because my extractions still had far too much tannin impurity in it, even after having waited 24 full hours for it to fall it, the extraction solvent still contained far more tannin than I believed possible, especially when using 99% IPA. Why for? 99% IPA contains 1% water, enough water to contain a large amount of tannin from the leaf. Having that figured out, I found that water washes of the extract right after all of the Isopropanol had evaporated out, leaving that last 1% of water in the bottom of the evaporation bowl I could pour that water off (as long as it had no smell of IPA to it) and reduce the amount of tannin in the extract. That wasn’t enough! I found that the extract STILL had lots of tannin in it… for a long time I would just have to continue refining the extract using Naphtha and Isopropanol regardless of having tannin in it. One problem with that though, as I was washing the extract and it became a lighter and lighter color I found that at some point it started to get darker and darker. Scratching my head…. What? Turns out, if you have lots of tannin in your extract and you continue washing it with solvents trying to make it get lighter and lighter it will at some point start to get darker with each wash and if you keep on trying to make it get lighter will eventually wash out every bit of the salvinorin and have nothing but light brown colored tannin in the glass which becomes much darker upon drying. Argg…
I learned that lesson the hard way. The tannin was causing me loads of problems and I didn’t have a way around it. After waiting for the tannin to settle out of the extraction solvent I tried to add another step by pouring the fluid through several layers of coffee filters. The filters worked, they loaded up with so much tannin that I had to change them out several times because the clogged up so much with tannin. But even then, tannin was getting through the coffee filters, even when stacked three ply and running the fluid through them several times over. Still there in fairly high quantities no matter how hard I tried to get it out. The only answer I could come up with next was to wait 12 hours for the tannin to fall out of the fluid, pour it off into a new container and wait another 8 to 12 hours all over again, pour it off, wait another 8 hours and pour it off of the tannins which continued to settle to the bottom of the container again. Now, that’s lots of work and lots of waiting, not a good answer but it helped reduce this contaminate by going through those extremes. Then all I had to do was remove most of the lipids with small washes of 99% IPA and then dump all of the extract into 100 ml of Acetone and wait for the remaining tannin to settle out. From there, the tannin was out (*so I believed) and all laying in the bottom of my 100 ml jar of Acetone which I could then pour off and have an amount of high purity salvinorin, depending upon how much of the waxy lipid and Chlorophyll I had prior removed with Naphtha and IPA washes.
*Believe me, simple things can be a huge block… even with the purity confirmation step I started using I later found that my extract still had tannin in it. Arggg again! I didn’t know that the Acetone had to be completely clear without any hint of cloudiness in it before pouring it off of the tannin. Assuming my extract was very pure just because it was white and that I had (thought) I confirmed it by pouring the salvinorin into Acetone and waiting 12 hours before pouring it off again. It was obvious to me at the time the slight cloud in the Acetone was just because the salvinorin was in it, causing it to cloud. WRONG. If there is any cloud to your Acetone, whether colored or not that’s tannin! Sometimes it takes a full day or longer for it to all fall out to the bottom of the glass. After two years of struggling with extractions every weekend spending many hundreds of hours trying to perfect this “simple” extraction method I finally found the way to do it and the right balance to come up with an extraction method which works very well.
After another year of extractions I added another step to the process, right after the Naphtha washes and then drying the extract I found that warm water washes of the grainy solids if crushed finely enough would dissolve most if not all of the tannin left in the extract and that by doing so I did not have to do the multi-stage pour offs of the extraction solvent three times over or more which saved me lots of time. As you can see, tannin is the big block in Salvia divinorum extractions if you want to obtain some fairly high purity extract, but if you incorporate all of the steps I have spelled out in my rather lengthy extraction Tek you can get it all out and if you then grow crystals with your extract end up with 98 plus percent purity salvinorin crystals, now that’s lab grade and lab grade without using a lab! Of course, you need one to confirm it!
Go to this link to see my collection of extraction photographs on yahoo: http://photos.yahoo....salvinorin2003/
I just received word from a chemist that he has refined the process further using other solvents to remove lipid fats which work better than Isopropanol. I have heard this same report that xylene is superior to IPA two years ago from from another source, so although I have not tried it myself I believe the report..
Here is a quote:
After the naphtha washes, toluene or xylenes will remove more colored impurities from the salvinorin that naphtha leaves behind, almost eliminating the need for washing with isopropanol.
Xylenes or toluene are better than isopropanol for the follwing reasons:
They are less dense, so the crystals fall to the bottom of the container faster for easier separation.
They are drier so less water that can ruin the salvinroin-A by ester hydrolysis is added
They dissolve less salvinorin-A, so the yield is higher.
They evaporate more quickly.
Posted 02 April 2005 - 01:07 PM
Posted 02 April 2005 - 07:01 PM
Posted 04 April 2005 - 06:05 AM
Also, archiving the pics is probably a good idea, I don't know how long the hosted site will be up.
Posted 04 April 2005 - 08:08 AM
Posted 05 April 2005 - 02:49 AM