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| | Posted on Tuesday, July 01, 2003 - 03:10 pm: | 
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W A R N I N G S
Before trying this process, inform yourself of the potential dangers of trying to smoke the extract itself by going to Daniel Siebert's cautionary page. - Please avoid smoking the straight extract, logistical problems involved in doing this could result in serious problems.
Acetone is very flammable. Educate yourself as to proper organic solvent handling techniques. Avoid risking sparks from metallic utensils, desktop or computer fans, and don't try to evaporate it in closed areas.
Note:
The following process is a compromise that trades efficiency for purity, to get as clean an extract as possible without loosing too much efficiency. This process will yield an extremely potent extract and the salvinorin can be very close to pure. It WILL BE far too strong to attempt smoking it. Use this process to enhance leaf and be very careful to keep track of how much leaf is extracted, and how much leaf on which the extract is deposited. Modifying the process by using a lower temperature solvent, or shortening the soak time can produce a purer extract, but at a greater cost of efficiency. In other words, more salvinorin will be left in the leaf. As written, this process will probably leave between 15-20% of the salvinorin in the leaf.
The Process:
When using this method without crushing your leaf up, or flattening it down into the bowl, you will probably need about 10 ml of acetone per gram of leaf. You may be able to use half has much solvent, or less, if it is crushed up enough to be in flattened layers, rather than in bunches of crinkled up leaf. Also, with this process you can use as much leaf as you want.
Crush your whole (dried) leaf to a course consistency to reduce the amount of solvent needed. It doesn't need to be powdered. The purpose of crushing is to reduce the volume, so that a small amount of solvent will cover the leaf. Whole leaf can be used if desired.
Put your leaf in a stainless steel, ceramic, or glass dish and put it all in the refrigerator. It should be cooled down to as close to 35 degrees F. as is possible.
Put your Acetone in the refrigerator as well. Again you are aiming for around 35 degree F. Please be very careful to properly label the acetone so no one mistakenly consumes it. This seems unlikely, but stranger things have happened.
Soak the crushed leaf in the acetone that has been cooled down to 35 degrees F. Soak it for no more than two and a half minutes, stirring continuously. (Reducing this time further trades yield for purity. A 10-30 second soak may be ideal if crystalline salvinorin is desired.)
Quickly decant the now greenish solvent and set it aside. (If minimizing soak times, solvent may not be greenish, as fewer impurities are solvated. This is OK.) Add fresh cold Acetone and soak it for three more minutes, (or less, if desired for purity) stirring continuously. Quickly decant it and keep the two extractions separate, you can combine them later. Generally keeping the two extractions separate is a good idea. The first is usually far cleaner than the second. If you are making enhanced leaf, feel free to combine the two extractions.
Let the (now possibly greenish) Acetone sit for several hours to let impurities fall out of it. You will find some fine greenish brown sand-like material in the bottom of the container. Carefully pour out the Acetone, leaving the stuff on the bottom behind. Save this sand-like material for further extraction, just in case some of the salvinorin was left behind.
You can now either add all of the Acetone right back to some finely crushed leaf, or evaporate it completely out in a glass bowl to see what you got. If you choose to evaporate it out without adding it right back to leaf, you will likely see a crusty crystalline-like extract, green, but very potent! Using this formula on 30 grams of leaf you will likely extract about 250 mg of crude salvinorin. This dry extract may contain as much as 75 mg of salvinorin (Depending upon your leaf.) This is a purity of about 30% for two combined extractions, but, the purity can be either a little lower, or much higher. There are too many variables to guaruntee an exact concentration. As a general rule, the second soak will reduce the purity far below what a single soak can do, but it increases the efficiency so much that it might well be worth doing. Don't attempt to smoke this material as it is far too potent. I only evaporate it all of the way down to look at the quality of the extract! and then re-dissolve the extract into Acetone and use it to enhance leaf. If you extract 30 grams of leaf and add it back to 2.5 grams of leaf, your will have about 2.5 grams of 10X, considering inefficiencies. A moderate dose is about 50 mg of this 10X leaf. A strong dose of this leaf is about 100 mg.
Note: When performing this extraction on large quantities, one might want to put the leaf, solvent, and utensils into the freezer to chill. Refrigerating the acetone will keep it cold, but mark it clearly so as to prevent accidental consumption by unwitting persons. Better yet, have a separate refrigerator AND clearly mark it as acetone. Freezing the fresh leaf will help rupture cell walls, making the salvinorin more easily extractable. It may also turn the fresh leaf into mush.
Once you have done this process to your whole leaf once, it cannot be done again without excessive black wax. There is probably 15 to 20% of the salvinorin still left in the leaf, you can make a much longer soak to get the remaining out, but it won't be nearly as clean. You can dry it and try it again later, but be warned that you will get lots of waxes.
Caution:
Be sure that your enhanced leaf is completely dry with no hint of Acetone smell before you attempt to use any of it! Drying might be accomplished in open air by spreading it out into a thin layer in a glass pan for 24 hours. Don't heat it in the oven, as this could ignite the acetone vapors. In fact it is a good idea to have a well ventilated outdoors spot to evaporate off the acetone. I have found that salvinorin can be destroyed at much lower temperatures than what is commonly stated in different information sources on the net. Especially when in solvent. If you must heat it, keep it at or below 100 F. This may seem extreme, but I have seen the salvinorin crystals disappear out of solvent to never reappear when heated to only 140 degrees F.
Don't get this extract on your hands and touch your face, it can cause skin to puff up, turn red and then dry in sensitive individuals. Soap and water will not cut it, you must wash your hands with solvent to remove it.
Cleaning up your extract:
It should not be necessary to further clean your extract when using the above process. However, there are a few additional steps that may be desirable to some persons. The extract can be further cleaned or refined by using just Naphtha, or Rosinol lighter fluid. Naphtha is superior to any other solvent when used to clean up an extract from this process because salvinorin is almost insoluble to Naphtha (compared to other solvents) and the green or non-salvinorin portion of the extract is extremely soluble to Naphtha. Although the extract from the above process is pure enough as it is, a Naphtha clean up can yield some very white salvinorin. (When doing very short extractions with cold acetone, a follow up cleaning step such as this is generally not needed in order to achieve crystalline salvinorin.)
When I did my first extraction using this method with 200g of leaf, I had let the extract completely dry and then put all of my dry crusty crystalline extract into about 30 ml of Reagent Grade Methanol. Immediately, the Methanol took on a dark green color and I could see crude salvinorin that contained lots of small crystals fall to the bottom of the container. Because of this, it was obvious that I had some highly purified extract to begin with. Although Methanol will work fine to remove the green, I should have used Naphtha instead of Methanol because salvinorin is far less soluble to Naphtha. This way, I loose less of the salvinorin to the solvent when I later pour it off from the salvinorin concentrate laying in the bottom of the container.
Naptha is also used in a process called partitioning (washing). It is used to clean up extremely impure extracts that contains so much chlorophyll that the extract appears to be made of black wax. This is the kind of extract that you will get if you try to extract from powdered leaf for more than just a few seconds with either Acetone or Isopropyl. You can also get it if you soak whole leaf in either of these solvents at either room temperature, or for too long a period of time. If you were to use the partition process to clean up a Salvia Divinorum extraction, you would first completely dry your extract out and then reconstitute it with 100% Methanol. Then, after completely dissolving your extract in it, you would mix the Methanol with an amount of water that would add 20% to its total volume (80% Methanol, 20% water). This is then mixed with an equal volume of Naphtha inside of a glass container called a separatory funnel. A separatory funnel is just a cone shaped seala! ble glass container that has a drain valve on the bottom. The partitioning process is used to remove an undesired component of one solvent by transferring it into the other. The whole sep funnel with its two layers of solvent is agitated, or shaken, to get the two solvents to temporarily mix together, something that they normally won't do. The solvents will separate into two distinct layers again, which could take several hours, days, or longer. The bottom layer of solvent is then removed and saved by opening the valve in the bottom of the container. The lower layer of fluid is the one you want to keep. You then evaporate off all of the Methanol and you should have a much nicer extract, at a cost, since you will loose some of the salvinorin to the naptha.
If you have partitioned your extract, the larger portion of the lost salvinorin can be recovered out of Naphtha by doing a process called "back washing" the (green) Naphtha with a fresh mixture of Methanol/water, added right back to the Naphtha in the separatory funnel (After the Methanol w/salvinorin has been drained off). For those of you who haven't guessed, when Naphtha and Methanol/water are mixed together in a separatory funnel, the Naphtha floats on top of the Methanol. Adding water to the Methanol increases the polarity of the methanol, making it immissible with Naptha, otherwise they will mix. If you were to try to add straight Methanol and Naphtha together, they would readily mix and no partition between the solvents will occur.
Cleaning up your dry extract using methanol or isopropyl:
Methanol can be used to clean up extractions directly (as opposed to cleaning them with naptha, then cleaning the naptha with methanol), but some of salvinorin is lost to the methanol because methanol will hold at least 3.15 mg per ml. Plain old 99.9% Isopropanol (Isopropyl) can also be used for cleaning up an extract and would be better than Methanol because it will saturate with about one fourth the amount of salvinorin per ml. Acetone would be the worst solvent to use for cleaning it up, it can hold at least 23 mg of salvinorin per ml. Keep in mind that you can't easily clean up the extract when using the quick whole leaf extraction process unless you first separate off the sand-like layer of particles that you will also extract out with the salvinorin. I still don't know what it is, but it isn't salvinorin A. Also, even using the two step process (When combining all of the Acetone together) you may get plenty of green, but it won't be so much that looks black. Aged lea! f that is six or more months old (the longer, the better) seems to be much better for this use, as it seems to extract out much less chlorophyll when using this quick process. A traditional 'cure' designed to destroy chlorophyll in smoking materials may also help with obtaining a cleaner extract.
Crystallization Notes:
One of the tricks that people use to grow crystals is to warm Methanol up and then add crude salvinorin to it. Because Methanol will hold much more salvinorin when it is warm then when it is at room temperature, the crystals slowly start to form as the liquid cools. In some circumstances salvinorin will just drop out of the fluid in a crude form, without crystallizing. Sometimes you need to seed the fluid with a crystal from a previous extraction, this can kick things off. Even so, I have seen salvinorin just drop out of the fluid as a non-crystal substance, even as white or light-green flakes. It can look like small sandy particles, flakes, a fine sludge, or crystals. It may be greenish, grayish, white or translucent with a yellowish green tint, depending on the type and quantity of impurities. One of the most pronounced things about salvinorin in solvent such as isopropyl, ethanol, or methanol is that it loves to stick to glass. In crude form, it will usually stick to ! the glass, but can be easily swished away by jiggling the solvent in the glass around. When I cleaned up my last quick Acetone extraction by pouring the dry extract into Methanol, the salvinorin that fell out into the bottom of the small 50 ml glass container was almost all crystalline, mostly greenish translucent crystals, but the crystals didn't stick to the glass at all, until I poured all of the Methanol out, then they just all stuck together to form a greenish gray sludge because they had not dried. They didn't look like crystals at all after I removed the Methanol. One of the methods used to keep crystals from adhering together is to pour out the Methanol, or what ever you used to grow them in, and then pour in a small amount of Naphtha to keep the crystals from sticking together. Then, you can more easily separate the individual crystals for drying, since Naphtha doesn't like to hold salvinorin, it will just evaporate off without dissolving your crystals away.
Notes about Acetone and Black Wax:
Ending up with black wax doesn't mean that your extract is ruined. It isn't. You just won't get the purity that makes enhanced leaf easier to smoke. For some, this is important. A regular extraction with 99% Isopropol alcohol isn't bad at all if your making some 5X, at that concentration it isn't hard to smoke, but go higher and it gets too sticky. For making your own 10X you need to get the salvinorin out without the gunk.
Making tincture
If reconstituting extracted salvinorin A into drinking alcohol keep in mind that ethyl alcohol holds only 1.8 mg of salvinorin A per ml. For comparison's sake, Daniel Siebert's tincture is said to contain about 1.36 mg of Salvinorin A per ml. It might be useful to aim for 1.4 mg per ml, and then dilute this to 50% alcohol in an aqueous solution. This will allow fairly rapid buccal absorption without the tissue damage that can be caused by 195 proof liquors such as Everclear. Keep in mind that 80 proof (40%) alcohol is common, and 80 proof vodka is the easiest, cheapest source of drinkable ethanol for most persons. As alcohol holds 1.4 mg salvinorin per ml, and water holds practically none, and a ml of 80 proof vodka holds only 40% ethanol, one might presume 1 ml of 80 proof vodka would hold .56 mg of salvinorin. An ethanol / water mix is likely to have different solubility characteristics than the average of water and alcohol though. Refer back to how adding 20% wate! r to methanol suddenly made that substance immiscible with naptha. It should be easy to take pure salvinorin crystals and calculate how much dissolves per ml, then aim for 50% of that (to prevent spontaneous crystallization in the solvent). I lack these numbers however. Email me if you find them.
Solubilities:
It has been suggested that a warm or hot water pre-wash of dried salvia leaves could remove as much as 1/3 of their salvinorin content. Generally a pre-wash is not required, and is not recommended. However if you feel the need for it, use cold water in order to err on the side of caution.
The data for the following table was collected using 15 grams of solvent for each gram of salvia leaf. Each involved a 16 hour soak at approximately 27 degrees C. All weights given are in gram units.
Salv. A, mg/ml @ 27C +/- 10% Solvent starting weight of leaf salvinorin extracted ratio of leaf to salvinorin extracted
acetonitrile .6 .12 .2
isopropyl alcohol 91% 4 .18 .045
acetone 2.7 .19 .07
ethyl acetate 2.8 .13 .046
dichloromethane (DCM) 3.3 .16 .048
Acetone and isopropyl alcohol are at least as useful solvents as other more difficult to acquire chemicals. Acetone is appears to be significantly more effective. Acetonitrile is very effective, but very toxic and more difficult to acquire.
{Editor's note: These solubilities were taken from the 'net. I've not attempted to verify them. A claim has been made that ethyl acetate should be a better solvent than is depicted here, but I'm not sure if this is true or not.]
salvinorin A solubilities, mg/ml @ 27C +/- 10%
solvent capacity comment
acetone ~23 best solvent choice identified thus far
methyl alcohol 3.15 ie. methanol
ethyl alcohol 1.28 else where in this article this number is reported to be 1.8, anyone know what the real deal is?
isopropyl alcohol ~0.74 this low carrying capacity indicates that this might be better used for cleaning the crystals rather than as an extraction solvent
cold water negligible keep in mind that as water warms, it carries significantly more salvinorin
Larger crystals were formed by the solvents capable of holding more mg/ml. It is interesting to note that ethanol has about the same solubility at -3C as at 27C. That is to say that changing the temperature seems to have little effect on the solubility of salvinorin in methyl alcohol. Also note that as a general rule, the slower a warm solvated chemical is chilled, the larger the resulting crystals.
Please note that the presence of other impurities, such as those sometimes co-extracted from leaves, can vary the solubility significantly, and often making crystallization difficult.
Standardized Extract
Short story: Dissolve a measured quantity of Salvinorin A in a solvent, and then absorb it onto a measured quantity of crumbled salvia leaves. Evaporate off the solvent, and it is done.
Thorough explanation: To make salvinorin A enhanced leaf that contains 15 mg salvinorin A per gram of leaf, dissolve 12.5 mg pure salvinorin A in 1 ml of warm acetone, and then add 1 gram of crumbled salvia leaves and stir. The leaves will absorb the salvinorin A-containing acetone. Place the container in a well-ventilated location and wait for the acetone to evaporate off. Stir the leaves occasionally during the evaporation period. Make sure that the acetone has evaporated completely--there should be absolutely no smell of acetone left on the leaves. This presumes that an average of 2.5 mg of salvinorin A per gram is already present in the leaf.
The amount of salvinorin A to use will vary depending on the salvinorin A content of the leaves that it is being absorbed onto. If the leaves are of average potency, containing 2.5 mg salvinorin A per gram, then you would deposit 12.5 mg salvinorin A onto them to bring the concentration to 15 mg per gram (as in the above example). Of course, one can standardize the leaves to other concentrations as well. The more precisely you know the salvinorin A content of the leaves, the more accurately you can standardize them. I use very pure salvinorin A for this procedure. If you are using salvinorin A that is not perfectly crystallized due to remaining impurities, you will need to take into consideration the percentage of impurities when calculating the amount of material to use. The same technique can be used to deposit salvinorin A onto other types of leaf.
For instance if deposited back onto salvia leaf that has had the salvinorin A removed, standardization becomes somewhat simpler. For each gram of leaf, deposit 15 mg of salvinorin A, and the leaf is standardized to 15 mg per gram, with no guess work as to what the leaf contained in the first place. The same holds true for garden sage (S. officinalis) which has no salvinorin A by default.
Smoking leaf that contains more than 15 mg salvinorin A per gram is strongly discouraged unless the individual doses can be accurately weighed. At this concentration, the amount of smoke produced provides a certain amount of safety because it makes it difficult for a person to accidentally inhale too large a dose in a single inhalation.
Caution: Light will begin to decompose Salvinorin in a few hours while dissolved in acetone. Alcohols are far less of a problem when exposed to light.
************PLEASE READ!!!************
This information is provided for research purposes ONLY! If you decide to ignore our warning and use this information to attempt to produce salvinorin and you are hurt in any way by either the process itself, chemicals used in said process, or by consumption of salvinorin or any byproduct of said process, WE WILL NOT BE HELD RESPONSIBLE!!! |
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