i found this on another forum, can't post links since against the rules, but got some nice infos and pictures in it
First a "quick" introduction
Quote:
Salvia Divinorum salvinorin Extraction and Refinement FAQ. January 1, 2006
By Christosphere
Zitat:
This extraction and refinement method was worked out and written by a non-professional, I'm not an organic chemist and don't work in a field related to botany or chemistry. The solvents mentioned in this document are very flammable and can be easily ignited by red hot surfaces, open flame, electric or static spark! Avoid risking sparks from metallic utensils, desktop or computer fans and don't try to evaporate solvents in closed areas. Do not use stirring utensils, containers or seals which can react with solvents as any contamination by plastics will completely ruin the extraction which then must be thrown away.
This document does not contain enough information to know how to safely handle solvents or their proper use for the manufacture of human consumable products and is not intended to imply that anything produced by this process can safely be used as a human consumable food or drug. The use of either crude or refined salvinorin as a drug should never be attempted, it is far too potent to eye ball a sub-milligram dose of salvinorin which can only be accurately done if using an analytical balance with accuracy within a tenth of a milligram or better costing many hundreds of dollars or more.
Salvia divinorum extract is an extremely potent and intoxicating psychotropic substance. Individuals seeking info on the possible negative effects of attempting to directly smoke or dose with either crude extract or refined salvinorin should read the warning at http://www.tinyurl.com/6urcj How do I extract Salvia divinorum leaf, should it be whole, crushed or powdered?
When I first started extracting Salvia divinorum leaf with acetone I found that it didn't seem to make any difference whether the leaf was whole, crushed or even finely powdered, regardless I found that salvinorin was extracted from leaf from whole to finely powdered with the same efficiency. Since acetone worked so well with whole or crushed leaf my assumption was that most, if not all of the salvinorin was coating the outside of the leaf instead of inside the leaf, either that, or acetone was somehow able to efficiently draw the salvinorin out of the interior leaf membranes. Daniel Siebert recently published a paper confirming my belief that salvinorin is concentrated on the outside of the leaf, because of this it isn't necessary to powder the leaf to be able to efficiently extract salvinorin using any solvent which salvinorin can be dissolved into. When I extract large amounts of dried leaf with acetone I usually just hand crush the leaf as fine as I can and then add enough solvent to completely cover the leaf with an extra couple of inches of solvent over the top of the leaf. Average potency Salvia leaf contains close to 2.5 mg of salvinorin per gram of leaf, high potency Salvia has been reported to be as high as 4 mg salvinorin per gram of leaf (although I have my doubts this is true).
The solubility of salvinorin in acetone at 27 degrees C. has been reported to be 23 mg per ml of acetone .74 mg for isopropanol and 1.28 mg per ml of ethanol. On this basis 100 grams of Salvia leaf should only need a few ml of acetone to extract the salvinorin but that amount of fluid is far too little to be able to completely cover finely crushed leaf! If the leaf is finely powdered to the consistency of flour you might want to calculate the amount of salvinorin in the weight of powdered leaf to determine the amount of fluid needed but otherwise I wouldn’t even worry about it, especially if extracting your batch of leaf two or three times over as I recommend. Although Salvia divinorum leaf does not require fine powdering to extract it, if you powder your leaf you can use far less solvent to extract the amount of salvinorin contained in the leaf but to be safe I like to use three or more times the amount technically required, especially when extracting leaf with either ethanol or isopropanol which salvinorin is far less soluble to compared to acetone. Alcohol extractions will yield just as much salvinorin as acetone extractions but always be generous with the amount of solvent needed when using either ethanol or isopropanol which will hold far less salvinorin per ml compared to acetone, requiring more fluid and longer extraction periods.
Is there a simple way to make enhanced leaf?
The following is as simple as it gets to make a gram of 5X enhanced leaf
(~12.5 mg salvinorin per gram of leaf):
1. Pour enough room temperature acetone into a glass container to completely cover six grams of finely crushed Salvia divinorum leaf and stir for three minutes or longer.
2. Pour acetone off of the extracted leaf into a glass bowl containing one gram of un-extracted finely crushed leaf and evaporate all acetone while leaf is present in it, mop up all of the residues from the sides of the container with the leaf as the last of the solvent evaporates out.
3. Once every hint of solvent smell is gone from the leaf, Wha-la! Enhanced leaf. Store out of the light, cold storage is better than warm, especially a freezer to assure many years of full potency.
Note: I like to use an extra amount of Salvia leaf to make up for possible extraction inefficiencies. In this simple method six grams of leaf are being extracted and placed back on one gram to make 5X leaf. Since a total of six grams is being extracted to place back onto one gram of leaf the total amount of leaf used is 7 grams to make one gram of 5x which should be every bit as potent as standardized 5x leaf, more than likely closer to 6x. Want to make something stronger using this method? Not recommended because of the increased amount of waxy lipid compounds placed back onto leaf in higher concentrations any more than a ratio of 6 to 1 is about as high as you can go without ending up with a very gummy and harsh burning leaf which produces too much smoke for most people to hack.
I want to make my own low smoke extra salvinorin infused standardized leaf, how can I do that?
This is a brief summary of the lengthy extraction write below it without the water wash of the dried extract (either prior to or following the naphtha washes) or the extra purification process of using 99% isopropanol. This method of refining salvinorin is a reasonable equivalent to true standardized leaf but unless extreme care is taken to assure the all of the tannin has been removed from the extract will not approximate standardized leaf. True standardization of enhanced Salvia divinorum leaf requires knowing the exact purity of the salvinorin which requires more sophistication than found in most homes however this method will work to produce 80% to 90% pure salvinorin (with experience) and is fairly easy to do using the methods outlined below.
With extra care salvinorin which is up to 98% pure can be produced through the refinement methods outlined in this document but unless you have a real need for high purity salvinorin is not worth the extra time and expense needed to produce it. Lower purity extract can be used to enhance leaf which is every bit as potent as a true standardized leaf by simply using more extract to make up the difference for being impure.
A rough approximation works very well for this and can easily be calculated by simply extracting from a given weight of dried leaf which is then deposited on a fractional amount of dried leaf plus 15-20 percent more extract than the strait math indicates to use. For example, if having extracted from 100 grams of dried leaf (oven dried at 125 degrees F. first to remove moisture) one might assume that amount of leaf could make 10 grams of 10X enhanced leaf. Due to processing losses you may only be able to make 8 grams but those eight grams should be every bit as potent as a true 10X standardized leaf because you are making up for common extraction losses. You can't claim a true standardization, but at the same time make something just as good, especially if you have remove most of the waxy contaminates from the extract. When most people buy "standardized" most are only after a guarantee of a minimum while at the same time wanting to be able to gauge how much material they need to smoke for a given effect so be careful not to put too much refined extract back on the leaf. Daniel Siebert at www.sagewisdom.org recommends no more than 15 mg of salvinorin per gram of leaf as a maximum amount but to make 10X leaf requires more. Although some individuals are attracted to higher X factor enhanced leaf believing that more is better, the truth is 5 to 6X strength leaf made by infusing ~15 mg into a gram of leaf is plenty potent enough and far less problematic to individuals who might either be new to Salvia or who are not taking enough care to accurately measure the amount of material they are smoking.
Warning: Do not evaporate acetone in closed areas (inside your house or garage). Beware of static or electrical spark, open flame (water heater pilot light) or red hot surfaces which WILL ignite vapors from the fluid which can result in the destruction of your and others homes, permanent disfigurement and worse... death. Sounds overly stated? It isn't.
Here is a simple outline of the process I use. This outline does not match number for number of the more in-depth and detailed write below it but gives a fairly strait forward view of the process:
1. Dry leaf.
2. Crush.
3. Soak leaf in acetone for 3 minutes, stir, save and pour off and save.
4. Repeat 3 times.
5. Discard leaf.
6. Add all acetone together, stir, let settle for 12-24 hours (the longer the better but in a relatively dark place away from strong light).
7. Pour off the acetone into a separate container being careful not to stir up the fine tannin particles in the bottom, save the acetone and discard residue on bottom.
8. Evaporate the acetone completely out, do this in a relatively dark place away from direct sunlight. Complete darkness is preferred to minimize reaction with light which can destroy a portion of your yield.
9. Upon complete evaporation of the acetone naphtha can be used to remove the waxy non-active lipids and chlorophyll contaminates from the extract solids. To successfully remove most of these waxy compounds (AKA black wax) it is very important to crush all of the extract into as fine granules as possible while in the naphtha. Stir the fluid and extract well and then let sit completely still for an hour or longer to allow most of the fine particles of salvinorin enough time to settle to the bottom of the container.
10. Pour the naphtha off of the extract solids leaving the salvinorin residues which have settled to the bottom behind. (Save the naphtha, more will settle out after 12-24 hours).
11. Add more naphtha to the extract solids, stir, let set long enough to completely settle out again.
12. Continue washing the extract solids with naphtha until the fluid no longer changes color or continues to lighten with each subsequent wash of the extract, allowing enough time for the fine salvinorin particles to settle to the bottom each time.
13. When satisfied you have removed enough of the chlorophyll pour off every drop of naphtha and dry the extract.
The dried extract produced by the above process is fairly crude compared to what you can make through further refining as explained in the more detailed tech (below), regardless, the purity from this rather simple method is plenty high enough to make enhanced leaf which is just as good and low smoke producing as expensive 5x to 25x standardized leaf which you can pay from 15 to 50 dollars or more a gram for, depending upon the amount of salvinorin infused into it.
When enhancing leaf with the extract produced by this process be sure to completely dissolve all of the extract into either 99% IPA or any solvent of your choice which salvinorin is soluble and then pouring over a quantity of crushed leaf and evaporating. Be sure not to use too much solvent than needed to completely dissolve the extract while at the same time assuring that every bit of the extract solids have completely dissolved. Continue to stir the leaf as the last of the solvent evaporates out and mop up the light residues from the sides of the container with the leaf while still moist with solvent. By finely crushing the leaf and thoroughly mixing afterwards you can average out hot spots created by using the leaf to mop up the high potency residues.
To approximate how potent your enhanced leaf will be, divide the amount of leaf extracted in grams by the amount of leaf you are infusing the extract into and subtract 10-15% for a rough "x" factor estimate which should be every bit as strong if not more potent than true standardized leaf.
The following was written for 100 to 250 gram extraction of dried Salvia divinorum leaf to make high quality Standardized leaf:
WARNING: DO NOT ATTEMPT TO USE CRUDE OR REFINED SALVINORIN AS A DRUG. IT IS FAR TOO POTENT, ESPECIALLY WHEN IN CRYSTAL FORM. 5X Enhanced leaf is less than 1.5% salvinorin by weight.
This extraction and refinement method will work for any amount of leaf, if using 25 grams of leaf instead of 100 grams scale the amount of solvent down by one quarter the amounts suggested. Nothing outlined in this extraction process requires extreme exactness to work and uses nothing more than simple kitchen utensils and household solvents. The following process can be used to extract and refine salvinorin into a purity that is in the high 90 percentiles:
1. Extracting leaf: Extract finely crushed leaf in a glass, ceramic or stainless steel container (no plastic bowls or utensils) using room temperature acetone three times over for 3 minutes each time completely covering the leaf with fluid each time, longer if desired. When using acetone to extract the majority of the salvinorin is extracted from the leaf in the first of the three 3 minute extractions, but I recommend extracting the leaf three times over just to be thorough. If using room temperature 99% isopropanol/IPA or 98% ethanol alcohol it is very important to thoroughly extract the leaf at least three times over for at least three minutes each time, longer if desired. Whether extracting with acetone, isopropanol or high proof ethanol shake or thoroughly stir the leaf into the solvent the entire time the leaf is in the fluid.
Note: This will work with whole unbroken leaf just as well. I prefer to crush my leaf to reduce the amount of solvent needed to completely cover the leaf. The amount of solvent needed to hold the salvinorin extracted from the leaf should always be in excess of the amount of salvinorin contained in the leaf. Regardless of which solvent you use to extract your leaf, if you finely crush the leaf by hand (not powdered) the amount of solvent needed to extract the leaf is only the amount required to completely cover the leaf with about an inch of fluid on top, especially when doing multiple extractions on the same leaf twice or more. Because the majority of the salvinorin contained in Salvia divinorum leaf is actually coating the outside of the leaf instead of inside whole or broken leaf can be extracted just as effectively as finely crushed or even powdered leaf, but when only moderately broken or whole requires far more solvent than needed on a solubility basis to completely cover the leaf.
If using 99% isopropanol or high proof ethanol to extract leaf, warming these solvents to 100-120 degrees F. will make them more soluble for salvinorin which is exactly but when heated will also produce far more vapors which increase the potential of fire from any kind of static or electric spark, open flame etc. which the vapors may reach to ignite them. However, room temperature ethanol will do the job just as thoroughly if soaking the leaf long enough and extracting several times over. If using ethanol to extract leaf I do not recommend 151 proof. Perhaps 191 Proof will work just fine for this kind of quick extraction, but I have never used it to know for sure myself. 99% medical grade isopropanol is much cheaper than drinking alcohol just as clean and although the solubility of salvinorin to isopropanol and other alcohols is far lower than acetone it will still do the job extracting all of the salvinorin out of the leaf at far less cost than high proof drinking alcohol.
2. Washing the leaf through again: This may not be necessary but to assure as much salvinorin possible has been removed from the leaf after completing the outlined number of extractions to the same batch of leaf thoroughly wash the wet leaf through once more with fresh acetone (or what ever extraction solvent your using) to further remove residuals. This is done to dilute out all of the old solvent remaining in the wetted leaf which could still contain some of the salvinorin. At this point your done with the leaf might want to place all of your previously extracted leaf into a jar with solvent for a long term extraction to get what ever amount of salvinorin that might have remained behind in the leaf which should be very little if any, especially if having used acetone. Re-extract the leaf as long as you like, but keep it in the dark to prevent any loss of salvinorin from long term exposure to UV light which can destroy a portion of the salvinorin while in solvents.
3. Combine all of the extraction solvent, filter tannin or wait 12+ hours to settle: Combine the solvent from all extractions and last washes, remove all leaf and fine leaf particles, filter tannin sediments from solvent through some kind of filter or let the solvent stand undisturbed for 12 to 24 hours to allow enough time for most of these sediments to settle out of the fluid. While waiting for the ultra-fine tannin particles to settle cover your container and store in a cool dark place to both reduce evaporation and to prevent possible losses due to interaction of light. Once you have waited at least twelve hours for the tannin to settle out of the fluid slowly pour the extraction solvent off of the fine brown tannin sediments which have settled to the bottom of the container, being careful to handle the container very slowly without jarring or sloshing the fluid to prevent the fine particles from being stirred up into the fluid. In large extractions where you are working with lots of fluid I don't recommend trying to pour out the last ounce or two of solvent out of the settling container because a portion of the tannin will usually flow out with the last of the fluid. Although, when leaving a small portion of the fluid behind a dilute portion of the salvinorin is still in it you can recover it by adding a few more ounces of fresh solvent to the fluid and vigorously swirling the tannin into the solvent for a couple of minutes to make sure to get any that might be left in it too, then waiting another 12-24 hours to settle again before pouring the fluid off again. Of course, you will have to leave the last bit of fluid behind the second time too.
Note: I have tried using paper coffee filters to remove tannin from the extraction solvent, but even after pouring the extraction solvent through paper filters stacked three ply several times a fair amount of the tannin particles were still able to get through the papers. A filter made of cotton balls in a glass tube might work better than paper filters, but I haven't tried it to know. Because the amount of solvent used will completely dissolve and hold far more than the amount of salvinorin extracted there is no fear of salvinorin falling out of the fluid, only the tannin impurity will fall to the bottom of the container, but these tannins should be saved for further processing later by swirling the sediments into fresh solvent and let to settle out once more be sure that none of the salvinorin was left behind in them.
4. Evaporating the extraction solvent: After the extraction fluid is poured off of and separated from the brown tannin sediments, completely evaporate the solvent. This is best done using a large flat pan so that the fluid volume will spread out much further than when using a bowl because the shallower the pan the larger the surface area of the fluid, speeding the rate of evaporation requiring far less time than if using a deep bowl. You can increase the evaporation rate even further by using a fan to blow air across the solvent with enough force to cause ripples on the surface of the fluid, but not so much airflow that droplets start taking to the air carrying away any amount of your precious extract. If you live in a buggy part of the world covering the evaporation container with a fine mesh screen which will both allow air to flow through and keep bugs out might be necessary. A full gallon of 99% isopropanol can be evaporated in under eight hours with this method and a gallon of acetone in four hours or less. Due to rapid evaporation of acetone, condensation from the air can cause an ounce or more of water to remain in the container which won't evaporate quickly and should be poured off because it will contain a considerable amount of tannin. Also, if you have extracted leaf using 99% IPA or 98% ethanol in addition to water from condensation you will have a percent or more of water remaining from the extraction solvent itself. This water is usually a yellow color due to tannins dissolved into it which is something you don't want in your extract, so once you have evaporated all of the solvent off and are left with only water pour it off, being careful that none of the green particles of extract go out with it.
Note: A large flat glass casserole cooking pan works very well to evaporate the extract into, the bigger the better. When the fluid level is being reduced by evaporation thin films of relatively high purity salvinorin are always deposited on the sides of the container. Acetone should not be used in jars that have lid seals unless manufactured for such use as acetone will melt many rubbers and plastics.
4.5 Removing more tannin from the extract while still wet: At this point you could remove more of the tannin from the extract if all hint of solvent has been evaporated off but the extract is still water wet from either condensation of water due to rapid evaporation of solvent, or wet from the 1% of water contained in 99% isopropanol. Keep an eye on the level of extraction solvent as the last of it is evaporating out and as soon as the fluid level gets down to 30 ml smell it to see if it has any hint of solvent left in it, if it doesn’t then scrape up all of the water wetted extract and place it into a an ounce or more of warm water and stir for a few minutes, breaking the particles up by hand as best you can by working all of the clumps out of the extract solids using your fingers. Depending upon how much tannin is in the extract and how much water is used the fluid can take on a light yellow to dark brown tint. Once your done working the extract into fine particles let the water set still undisturbed for an hour or for however long it takes for the particles which have been stirred up into the fluid to all settle to the bottom of the container and then pour the water off being careful not to let any of the solids flow out with it, add more water and stir the extract again. Keep doing this until the water no longer takes on any color and then completely dry the extract in an oven set to 125 degrees F. until no hint of moisture remains. Save all of the water used to remove tannin and check it in a few hours to see if more salvinorin has settled into the bottom of the container.
Note: This extra step to remove more of the tannin impurity by pouring in and stirring a an ounce or more of water into the extract will only work at this point if the extract is still moist and has not dried yet because once all of the water has evaporated out of the extract the lipid fats will congeal together to form coating around the tannin particles which will become a barrier to the water. However, if you have allowed the extract to dry there is still another point in the process where this can be done. The water washes of the extract can also be done after the naphtha washes, as long as you have completely evaporated all hint of naphtha from the extract solids prior to adding water. The majority of the extract which dries on the sides of the evaporation container can contain a substantial portion of the salvinorin extracted and if a crusty hard film which sticks to glass is without a doubt high purity salvinorin so be sure to scrape every bit of it off too. All of the waxy deposits on the evaporation container should also be scraped off and saved for step 5., if necessary using naphtha to remove these residuals from the sides of the container. It is important to remove all of the extract from the evaporation container so that it is completely clean as these films can contain a substantial portion of your yield.
5. Using naphtha to remove lipid fats and chlorophyll: Once every hint of solvent has been evaporated out and the extract is completely dry of moisture pour in four or more ounces of pure naphtha directly into the evaporation container (if already scraped out of the large evaporation container transfer all of the extract into a bowl so that you can work with it better). Completely dissolve all clumps of extract or wax into the naphtha so that only fine granules remain in the fluid. This may require crushing with a spoon while in the naphtha or working the extract between your fingers until all of the clumps are smoothed out. Next, pour all of the naphtha and every bit of the extract into a glass jar and thoroughly mix the extract into the solvent for a couple of minutes and after mixing set it aside undisturbed for two hours or more. What you are waiting for is for the ultra-fine salvinorin particles which were stirred up in the naphtha to settle to the bottom of the glass which can take a long time for most of them to fall out of the fluid. After the salvinorin particles have settled the fluid will become translucent, if at all cloudy the particles have not all settled out yet. After the salvinorin has settled to the bottom of the glass, slowly, taking great care not to let any of the particles flow out with the fluid pour the dark green naphtha off of the solids in the bottom of the glass. To continue washing the extract I like to work with smaller containers and recommend placing the extract solids into either a small shot glass or a 25-50 ml vial about one inch wide by two inches tall. Add more clean naphtha to the glass and mix the extract into the fluid for another couple of minutes and set aside for an hour or more before pouring off the naphtha again. Continue mixing naphtha into the extract solids and washing over and over (waiting for the particles to settle each time) until the fluid becomes a fairly light translucent green tint, at this point the naphtha has become ineffective for removing much more of the waxes and chlorophyll. Once the fluid stops taking on more color with each additional wash of the extract solids stop using naphtha. When done be sure to completely pour off every last drop of naphtha and completely dry the extract until no hint of naphtha remains.
Note: Since salvinorin is completely insoluble to naphtha but the dark waxy lipids from the leaf are fairly soluble to this solvent you don't need to worry about using too much, use as much as you like but take care to wait long enough for the ultra fine crystalline salvinorin particles to fall to the bottom of the container before pouring the fluid off. I have outlined using 25-50 ml at a time because I have found that working with smaller amounts of fluid is easier for me but larger amounts of naphtha can be used if you don’t mind the extra amount of time it takes for the particles to all settle. To check for the presence of these particles floating in the fluid shine a bright flashlight into the fluid from the top while viewing in subdued light and you should be able to see large amounts of extremely small particles of salvinorin slowly settling in the fluid, so slowly that you might not be able to see movement, but they are. Using several ounces of naphtha at a time might require waiting several hours for the majority of the salvinorin particles to settle to the bottom of the container, but when using a small one ounce glass most of them should settle in the first hour or so.
Do not use naphtha to remove fats from your extract unless you know for sure that the naphtha you are using will evaporate completely clean without leaving any amount of residue. Although, if continuing to clean the extract solids with 99% isopropanol these contaminates should be washed away I do not recommend using questionable purity. 99 percent isopropanol or 98% ethanol can be used in place of naphtha. These two Alcohols will do the job even better than naphtha but using them will remove some of the salvinorin from the extract each time you wash the solids, but no so much to be a problem if you use it sparingly enough. The solvent used to clean the solids can be evaporated and worked again to recoup the salvinorin lost to the washes, in ever diminishing returns, of course. The same with ethanol, this alcohol can be used in place of isopropanol but high proof ethanol removes more than twice as much salvinorin per ml as isopropanol and because of this, unless you want to go food grade all the way with your solvents I don’t recommend it.
If you have done a good job removing most of the tannin from the initial extraction and then removed as much of the fats as you can using naphtha followed up with water washes of extract to get the rest of the remaining tannin, the amount of dried extract from a 250 gram extraction of average potency leaf should weigh close to one gram and be over 50% pure with the remaining waxy impurities. Although they might not seem to be present if your extract is a grainy dry substance, if it is still green colored the waxy lipids are still there, even if it feels completely dry without any amount of sticky tack to it. At this point the extract is quite pure enough to use for making enhanced leaf without incurring additional losses through more processing so you can stop right here if you want to have maximum yield and assume the extract is close to or above 50% pure. The extract should be checked to make sure there isn’t any tannin remaining by performing the purity confirmation outlined in step 8 (below) of this document. Be sure to save all of the water used to remove tannin and check it in a few hours to see if more salvinorin has settled out of the fluid.
6.0 Making tincture.
Skip this step if you are not making tincture.
Dried extract which has had the majority of the waxy lipids removed by pure naphtha is perfect for making tincture, just dissolve as much of the extract as you can into 151 to 191 or higher proof ethanol drinking alcohol of any kind while at room temperature and you will have an effective tincture, the higher the proof the more effective. In my experience, removing more of the chlorophyll and lipid compounds by continuing to wash the extract solids with 99% isopropanol will at some point make the extract too pure for making an effective tincture if using 151 proof drinking Alcohol. When making tincture from high purity salvinorin without some of the other compounds from the leaf present in it should only be done when using extremely high proof ethanol such as 98%, but even then I believe an amount of the dark compounds from the leaf somehow helps sublingual absorption of salvinorin. If having extracted from 100 grams of dried leaf you should be able to make at least 5 to 6 ounces of 151-191 Proof ethanol tincture from that amount of extract. If you have extracted from enough leaf to make six ounces of ethanol tincture be sure to dissolve all of the extract into the drinking alcohol all at once instead of making each ounce of tincture separately, otherwise if using too much extract for the amount of Alcohol the excess salvinorin won't fully dissolve and end up in the bottom of the tincture bottle as a solid which can easily make a dose of tincture far too potent if a large portion of the fine solids are accidentally sucked up into a dosing dropper. However, there is one positive way to look at it if you find salvinorin solids in the bottom of your ethanol you can be assured that the ethanol contains as much salvinorin as can be dissolved into the alcohol but I would then pour the alcohol off of the precious solids and save them for the next batch.
Note: These are guesstimates; If using 191 Proof ethanol this alcohol probably won't hold much more than 1.0~1.2 mg of salvinorin per ml of fluid when at room temperature. High Proof 98% ethanol is reported to be able to hold close to 1.3 mg per ml of fluid. A chemist reported to me that he found that when a moderate amount of the waxy compounds from the leaf dissolved into 98% pure ethanol can hold much more salvinorin per ml. I have found when making my own tincture using 151 Proof ethanol and dissolving nearly pure salvinorin into that low of a Proof alcohol that the tincture was not at all effective without also having the dark waxy compounds from the leaf present in the tincture too. Perhaps the tincture was ineffective because I could not dissolve enough salvinorin into the 151 Proof ethanol (which is close to 25% water) or because some of the dark waxy compounds from the leaf are needed to help sublingual absorption, or both. Either way I have found that an amount of the dark impurities from the leaf was need for tincture made from 151 Proof ethanol to be effective.
7. Further purification: To further purify your extract begin washing the solids with very small amounts of 99% isopropanol in a ratio of no more than 1/3 dried extract to 2/3 isopropanol in a small 25-50 milliliter vial or shot glass until the extract is a light green to yellow tinted or white colored salvinorin. This is done by pouring in IPA and mixing the extract into it for a couple of minutes until the fluid becomes a dark color and then setting the small glass aside to wait for the fine crystalline salvinorin particles to settle to the bottom of the glass which can take an hour or more the first time. If having extracted from less than 100 grams of dried leaf the amount of 99% IPA used for each wash should be limited to about 25 ml per wash, if having extracted from 250 grams of leaf 50 ml per wash. Washing the extract solids with smaller amounts of isopropanol, regardless of the amount of leaf extracted will cause less of the salvinorin to be lost on a wash per wash basis but requires more washes of the extract solids. Regardless, using less fluid each time will cause the losses to be minimized and should be done this way to minimize the losses from this purification process. During the first wash of the extract with 99% IPA the fluid will likely become so darkly colored that even after the majority of the salvinorin particles have settled to the bottom of the glass it can be very difficult to tell where the layer of fluid ends and solids start in the bottom of the glass. Because of this remove no more than half of the volume of fluid before adding more isopropanol. This can be done by either using an eye dropper to remove the fluid from the top (don't dip too deep), or by carefully pouring half of the fluid out of the glass while closely watching under a strong light (without UV) to make sure none of the solids start to flow out with the fluid. When pouring the isopropanol off you probably won't be able to get the last third or more of the fluid out without also pouring some of the solids off too. Just leave that last third of the fluid in the glass and add more isopropanol to it because it will eventually dilute out anyway. Using an eye dropper to remove the fluid on top of the solids is my preferred method to reduce losses but is much slower than pouring.
Continue washing the extract by adding more IPA, stirring and letting the glass sit still long enough for the majority of the salvinorin particles to settle out of the fluid in cycles of removing the fluid and adding more until the solids which settle to the bottom of the glass are as light colored as you desire, the lighter the color the higher purity the extract will be. As the salvinorin becomes cleaner with each wash of the solids, the micron sized crystalline particles of salvinorin will take longer and longer to settle out of the fluid, when approaching high purity taking as long as three hours or more to completely settle after each wash when using a single one ounce glass, longer for larger capacity containers due to the increased amount of fluid. Don't pour the fluid off of the cleaned salvinorin in the bottom of the glass if the fluid has a cloudy look because this means that you still have lots of fine salvinorin particles floating or suspended in the fluid and you should wait for however long it takes for them to settle before removing the solvent. You can continue washing the extract until it is a light green color or all the way to white if you like, however this will increase your losses, up to 25% going as high as 50% if you don't wait long enough for all of the fine particles to settle.
Cleaning the solids to a white color isn't necessary because once the solids are a very light green tint (as long as all of the tannin has been removed too) the extract is a high enough purity to consider it well over 90% pure for use to enhance leaf, just use 10-15% more extract when lightly colored to make up for being less than completely pure. Be sure to save all of your isopropanol from the first wash plus as it can contain a quarter or more of your salvinorin, depending upon how much was used, how far you cleaned the extract and whether you waited for all of the salvinorin particles to settle before pouring off. If having extracted from 100-250 grams of leaf, use no more than 25 ml of 99% isopropanol per wash. You can use half of this amount of fluid per wash, just don’t use more. If extracting from one ounce of leaf (28 grams) no more than 8-10 ml per wash. Although salvinorin is weakly soluble to room temperature 99% isopropanol take great care to use as little as possible or you will loose too much salvinorin with each wash to the point of removing most of your yield if too much is used.
Note: Small amounts of 99% isopropanol can hold far more lipid fats and chlorophyll impurities than it can hold salvinorin on a milliliter basis and due to this when the extract is washed through several times with a few milliliters of this solvent more and more of the green is removed while the bulk of the salvinorin will remain behind. When waiting for the salvinorin particles to settle to the bottom of the glass about half of the salvinorin will fall out of the fluid in just 20 minutes because they are relatively large particles but the smaller and nearly impossible to distinguish particulates of salvinorin will continue to fall out of the fluid for three hours or more, although 80-90% of them will have settled in the first hour. To prevent large losses of your yield to the isopropanol washes of the extract you must wait for all of the extra fine salvinorin particulates to fall out of the solvent, waiting for the fluid to become completely clear is VERY important. Understand I do not mean colorless, the isopropanol can be from very dark shades of green to light yellow or all the way to white, but never cloudy before you remove the fluid or you will loose a significant portion of your yield. To see if the fluid is cloudy or not hold it up to a bright light, if you can’t see through the fluid like looking through dark to lightly stained glass then salvinorin particles are blocking the light.
8. Purity confirmation: Once your extract has been cleaned to the color desired and completely dry and free of any other solvent, you can check to make sure it does not contain any tannin impurity by dissolving all of your extract into 100 ml of room temperature to warm acetone. If after stirring the fluid for a couple of minutes it does not become a clear color wait 12 or more hours to see if tannin particles fall to the bottom of the glass. You don't need to worry about trying to dissolve too much salvinorin in 100 ml of acetone from a 250 gram extraction of leaf because that amount of acetone should easily hold close to four times the amount of salvinorin in the dissolved state which would be contained from that amount of average potency leaf, being able to hold approximately 2300 milligrams of salvinorin when at room temperature.
If the fluid appears at all cloudy after dissolving salvinorin into it this means that either you didn't dissolve the salvinorin into the fluid thoroughly enough, or there is lots of fine tannin present. Unless tannin is present and stirred up into the acetone it should be clear, it can be colored from a light yellow to a dark green tint if you didn't remove all of the dark green compounds but never cloudy before you pour the fluid off or something is wrong. If after 12 hours the acetone is still cloudy continue to wait, the tannin will fall out of the fluid eventually, taking as long as 24 hours in one case when I did it. When your ready to pour the acetone out for evaporation to net your tannin free salvinorin don't try to get the last few milliliters of fluid out of the glass because some of the tannin will come along with them, better to add more acetone and shake it up to dilute what ever remaining salvinorin there might be in the remaining fluid or mixed into the tannin sediments than to try to pour out every last drop of fluid. Of course, you will have to wait for the tannin to settle out again.
Here is a standardization procedure so that you can add salvinorin back to leaf. This came from a well known Salvia divinorum researcher explaining how to make 6X enhanced leaf:
The method is simple: 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 Wha-la! Here is a more detailed 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.
* 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 material that is impure, you will need to take into consideration the percentage of impurities when calculating the amount of material to use. Obviously, the same technique can be used to deposit salvinorin A onto other types of leaf.
I strongly advise against smoking leaf that contains more than 15 mg salvinorin A per gram 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. If you have a precision balance that can accurately weigh small doses, then stronger concentrations are preferable since the amount of smoke can be minimized without compromising safety.
Note: acetone is the best solvent to use for enhancing leaf because so little fluid is required to completely dissolve relatively large amounts of salvinorin, and evaporates fairly rapidly compared to Alcohol.
Is there a way to make a less harsh smoking enhanced Salvia divinorum leaf?
Yes, although this might actually make the leaf too easy to smoke. I have found that Salvia divinorum leaf is much easier to smoke when most of the chlorophyll and tannin has been removed from it. Here is how I make my own high quality standardized Salvia divinorum leaf:
The first thing I do is hand select Salvia divinorum leaf for quality, setting aside the stiff dark to almost black colored leaf in favor of the lighter colored soft green leaves. Once I have my pile of leaf to be made into incense I carefully hand de-vein the stem running through the center of each leaf being careful to keep the leaf in as few pieces as possible. When I have a full bowl of de-stemmed and de-veined broken leaf I then extract the leaf with a room temperature solvent such as acetone or 99% isopropanol several times to remove the salvinorin which is set aside for later processing. Because of the extra work required selecting the best leaf and de-veining them this process isn't meant to obtain salvinorin, but rather to condition the leaf to ready it for salvinorin enhancement.
Next, I take the spent leaf, having already had the salvinorin removed form it and re-extract the leaf but this time instead of trying to get the salvinorin out the extraction is for removing as much of the dark waxy compounds from the leaf possible. Once you are done pour every bit of the solvent off of the leaf and let it completely dry without a hint of solvent smell in the leaf and then boil all of the leaf together in a pot of hot water for a half hour or more, once the water turns brown pour it off and add more water to boil the leaf again. Keep doing this over and over until the water will no longer take on a brown color. When done pour all of the water off of the leaf and spread it out on a cookie sheet and dry in an oven set to between 125 degrees F. for however long it takes to completely dry, usually several hours in a convection oven. After the leaf is completely dry you can use it to make your own standardized enhanced leaf at what ever X factor you desire. When Salvia divinorum leaf is conditioned this way by removing most of the chlorophyll and tannin first the leaf will then readily absorb salvinorin dissolved into acetone when making standardized leaf.
If you have finely crushed leaf instead of large pieces you can process the leaf just the same, but I like to keep the leaf in as large and few pieces as possible because when drying in an oven they will shrink quite a bit. Also, I believe that large pieces of enhanced leaf are better than smaller pieces because it provides far more options for how it can be burned. The only thing is, when you have such nice big pieces of enhanced leaf you won't want to package it in small plastic bags which can easily allow the leaf to be crushed or broken further.
Extraction notes, insights to the process:
The solubility of pure salvinorin at 27 degrees C. in acetone is approximately 23 mg per ml of fluid, for 98% ethanol 1.28 mg per ml and for 99% IPA .74 mg per ml of fluid. For isopropanol extractions I like to use enough solvent so that it completely covers the leaf extracted and when using 98% ethanol or 99% IPA at least two thirds or more times of but when increasing the amount of fluid this allows the leaf to be easily and thoroughly mixed within the solvent when stirring. The amount of time the leaf is soaked in either solvent can be extended for as long as you wish, this will only help increase the extraction efficiency, however I have found that when extracting Salvia divinorum leaf three times over for five minutes each time with 99% isopropanol that it won't get all of the salvinorin out, usually leaving 10% the salvinorin behind which requires an additional long term soaking of the leaf to get the last of it out. When using acetone to extract leaf I have found that it will remove the salvinorin so efficiently that when re-extracting the leaf a fourth time over to check and see if any was left behind I have not been able to get enough additional salvinorin to be able to tell. If using isopropanol I do not recommend using anything less than 99% for this quick extraction method as IPA with large amounts of will increase the amount of time required to efficiently extract the salvinorin. 91% to 94% IPA might work for short extractions, but I haven't tried it to know but I can tell you that I have tried 70% IPA several times and found that with 30% water in it I found it to be useless for a quick extractions, only able to extract a waxy compound and tannin out of the leaf in the short amount of time I have outlined in this extraction tech.
This extraction process has three separate steps incorporated into it to remove tannin impurities, the first step will get most of it, the second step another portion and the last step every bit of it if you are careful. Waiting up to 24 hours for the tannin to fall out is better than 12. Be sure to keep extraction solvents in complete darkness the whole time while waiting for tannin to fall out because if the solvent is left out in bright sunshine you can loose a large portion of your yield due to the interaction of strong ultra-violet light while in solvent. Tannin impurities are a big problem, almost everyone has the same problem with tannin the first few times they try this extraction technique ending up with far more of it in their extract than they believed possible thinking that all of it must have certainly settled out of the fluid when waiting as many as 24 hours for it to come out of the fluid, but even after waiting a full 24 hours the tannin is still in there to some extent, especially if having used a solvent with any amount of water in it to extract the leaf. To deal with this common problem I have worked an additional step into the process to wash out tannin that remains in the extract after cleaning with naphtha (drying first) using water and then one more tannin removal step at the end of the process by dissolving the cleaned extract into acetone again and waiting 12-24 hours to see if more drops out of the fluid because at that point regardless of your best efforts you will likely still have some of it in the extract. Be careful not to touch your face or other sensitive areas of skin when working with Salvia divinorum wetted by solvent or when having residues from the extract on your hands. Something in the leaf can cause an allergic reaction and extreme drying of the skin which I believe is caused by the tannin in the leaf which is a very strong astringent which causes sensitive areas of skin to become reddened along with an amount of swelling and later flaking of skin which can last several days. I have never had a problem with the skin on my hands or arms but my face always has this reaction if I scratch my nose or rub my eyes when slight amounts of extraction residues or are present on my fingers this happens every time.
The reason I use naphtha to remove the chlorophyll and other waxy lipids from extract first before switching to acetone is because salvinorin isn't soluble to naphtha but the dark waxy compounds are. Unfortunately, after a few washes of the extract with naphtha it becomes ineffective for removing the last of the lipid and chlorophyll impurities requiring the use of another solvent such as 99 isopropanol to get the last of it. Although 99% isopropanol does an excellent job of removing the remaining dark waxy substances from the extract this solvent removes at least three quarters of a milligram of the salvinorin per ml of fluid when at 20 degrees C., more when IPA is warmer, less when cooler (more if you don’t wait long enough for the salvinorin particles to settle). Also, the solubility of salvinorin has been reported by an experimenter to be much higher in 99% IPA when large amounts of other compounds from the leaf are present which can result in a significant portion of your yield being removed with each wash of your extract if you use too much, so use it very sparingly. You can recover a large portion of the salvinorin lost to the isopropanol washes by completely evaporating the solvent and removing the dark lipid waxes using the same process over again with naphtha and IPA in much smaller amounts. Save all of your naphtha used for the washes because although salvinorin is insoluble to naphtha there are usually extremely small particles of salvinorin in the fluid which take much longer than an hour fall out of the fluid and can be found in the bottom of the container after 12 hours or more netting another 10% of salvinorin. Save all of the IPA used to wash your extract because it can be evaporated onto leaf to make 5X enhanced leaf or after evaporation reconstituted into drinking alcohol to make tincture, depending on how much salvinorin was removed through the washes. Be sure to scrape every bit of film from the sides of your evaporation container because high purity salvinorin films stick to the surfaces of evaporation containers whether stainless steel, ceramic or glass. This is one way to know you have salvinorin, because it sticks to these surfaces so well. To see photographs of a room temperature 99% IPA extraction of Salvia divinorum leaf and chlorophyll being removed from extract using naphtha and 99% isopropanol go to: http://www.erowid.org/plants/salvia/...raction4.shtml
and now the real part...
Quote:
Reduced Lipid Extractions Using Chilled Acetone
Salvia Divinorum Extractions Using Chilled Acetone. December 30, 2005.
By Christosphere
Zitat:
Disclaimer: This extraction and refinement method was worked out and written by a non-professional, I'm not an organic chemist and don't work in a field related to botany or chemistry. The solvents mentioned in this document are very flammable and can be easily ignited by red hot surfaces, open flame, electric or static spark! Avoid risking sparks from metallic utensils, desktop or computer fans and don't try to evaporate solvents in closed areas. Do not use stirring utensils, containers or seals which can react with solvents as any contamination by plastics will completely ruin the extraction which then must be thrown away.
This document does not contain enough information to know how to safely handle solvents or their proper use for the manufacture of human consumable products and is not intended to imply that anything produced by this process can safely be used as a human consumable food or drug. The use of either crude or refined salvinorin as a drug should never be attempted, it is far too potent to eye ball a sub-milligram dose of salvinorin which can only be accurately done if using an analytical balance with accuracy within a tenth of a milligram or better costing many hundreds of dollars or more. Salvia divinorum extract is an extremely potent and intoxicating psychotropic substance. Individuals seeking info on the possible negative effects of attempting to directly smoke or dose with either crude extract or refined salvinorin should read the warning at http://www.tinyurl.com/6urcj
A chilled acetone extraction uses exactly the same steps as for a room temperature extraction using 99 percent isopropanol (IPA) or high proof ethanol where the leaf is extracted three times over, then combining the solvent from all three extractions in one container together for a 24+ hour period of time to allow settling of tannin particles. When using chilled acetone the amount of time the leaf is in the acetone should be limited to about three minutes for each of the three extractions for a total of no more than 9 to 10 minutes in the chilled solvent.
In my experience the majority of the salvinorin will be extracted from the leaf in the first 3 minute extraction when using chilled Acetone but I recommend extracting the leaf three times over just to be sure. If the amount of time the leaf is kept in the chilled solvent is limited to ten minutes total the amount of waxy lipids extracted will be far less than if having extracted the leaf for a longer period of time. Longer extractions with acetone are not necessary, even when chilled using this process efficiently extracts virtually all of the salvinorin from the leaf in just two to three short extractions which upon tannin removal and evaporation will produce an extract which is very easy to refine using nothing more than a few washes with naphtha and 99 percent isopropanol.
When working in a room temperature environment pre-chilling both the leaf and the extraction container with the acetone together to a temperature no higher than 20 degrees F. will help keep the temperature below 40 degrees F. throughout the extraction. You want to start out cold and keep the solvent cold throughout the extraction, but when working in a warm room the temperature of the fluid can increase by 20 degrees F. to be as high 40 degrees F. while finishing up the last of the three extractions. This amount of temperature increase is ok, but no warmer than that and only during the last couple of minutes the leaf is in the solvent or you will begin to pull over additional waxy lipids in a hurry.
Due to the high solubility of salvinorin to acetone, even when chilled to zero degrees F. acetone is still far more effective for dissolving salvinorin from the leaf than room temperature 99 percent isopropanol or high proof ethanol alcohol, so don't worry about chilling the acetone that far down because your extraction efficiency will still remain very high when using zero degree F. acetone. If you are considering the idea of using chilled isopropanol or ethanol to extract leaf it won't work, I tried 99% IPA and found that it required four times the amount of time in solvent for one quarter the extraction efficiency of chilled acetone!
Extremely brief extractions of Salvia divinorum leaf of one minute or less with acetone chilled to close to zero degrees F., with exception of an amount of tannin extracted, will yield an almost wax free extract of high purity salvinorin. When extracting Salvia leaf for just one minute you might not get the majority of the salvinorin out of the leaf, depending on how well you agitate the leaf in the solvent, but you should get close to half of it.
At one time I had reported that chilled acetone extractions were less efficient than room temperature Acetone because when using 99% IPA to remove the dark waxy lipids from the extract I did not wait long enough for the salvinorin particles to all settle out of the fluid which was what really caused the losses and not due to the solubility of Acetone being too low from being chilled to zero degrees F.
The photograph below shows a chilled Acetone extraction that started at +5 degrees F. which warmed up to +15 degrees F. by the time it was completed which is fairly typical when working in a warm room, even if you have pre-chilled both your leaf and extraction containers together with the Acetone at the same time.
Shown in the photograph is the first wash of the extract with Naphtha, two washes with water and then four washes with 99% IPA to further remove impurities yielding white salvinorin. 99 percent isopropanol can be used to further clean the waxy impurities from the extract more effectively but will also remove a portion of the salvinorin with each wash of the extract solids. I recently developed another method which does away with isopropanol washes simply by pouring the extract together with the naphtha from the last wash of the solids together into a small dish and heat evaporating at about 125 degrees F. which causes the waxy chlorophyll and lipids to form a crust on top of the heavier salvinorin as it evaporates which can then be pealed away after hardening to expose the high purity salvinorin in the bottom.
The weight of salvinorin shown in the photograph of the scale is NOT representative of the extraction efficiency because when I did this extraction I did not wait long enough for the super fine salvinorin particles to fall to the bottom of the glass and unknowingly removed lots of salvinorin when using the IPA to remove the dark waxy impurities. I later recovered the salvinorin from the last two washes by completely evaporating the IPA and cleaning it once more using naphtha and more IPA which netted another 200 mg of salvinorin making a total of 525 mg of cleaned salvinorin from the 250 gram extraction, which is very good for average potency leaf. This doesn't include the salvinorin lost from the first two 99% IPA washes.
When removing lipid fats or waxes with 99% IPA the cleaner the salvinorin gets the longer it takes to settle to the bottom, taking an hour or longer to all settle to the bottom of the glass. If you have removed most of the dark green from your salvinorin and are left with a cloudy yellow fluid this means that you still have lots of super fine salvinorin particles floating in the IPA (as seen in the photograph below, the IPA was still cloudy) and must wait until the fluid is completely clear before pouring off the IPA. The fluid can be colored, but not so cloudy that you can't see through it as solvents which are fully saturated with salvinorin are never that cloudy and should be clear unless salvinorin particles are still floating in it (unless fine tannin particles are still present). Even if you have waited long enough for all cloudiness to settle out of IPA used to remove impurities from your extract be sure to save this solvent because something in the dark compounds from the leaf appears to increase the solubility of salvinorin to Isopropanol to be able to hold well over 1 mg per ml of salvinorin per ml of fluid, reported to some times be as high as 5 mg per ml by a chemist who had the use of an HPLC to test the solubility of salvinorin in a few different solvents. Whether the ability of IPA to hold that much salvinorin per milliliter was due to an actual increase of a solubility to IPA or whether it was caused by fine particles of salvinorin that were still floating in the solvent is something to consider.
The following image shows a chilled Acetone extraction at +15 degrees F. which yielded a total of 525 milligrams of cleaned salvinorin from 250 grams of finely crushed leaf.
The photograph showing 325 mg of cleaned salvinorin did not include the salvinorin later recovered from the IPA used to remove the dark chlorophyll and waxy lipids. Since Acetone is so wonderful at being able to quickly dissolve salvinorin from leaf the extraction efficiency itself was close to 100% but the total yield of cleaned salvinorin after reprocessing the IPA used to clean the extract (not shown) was close to 85%.
The loss of salvinorin to each wash of the extract solids with 99% isopropanol shown in the photographs above was greater than it should have been because I did not wait long enough for all of the ultra-fine salvinorin particles to settle out of the fluid prior to pouring the IPA off of the salvinorin which had settled to the bottom in the first hour. For maximum yield I should have waited up to three hours for the fluid to completely clear of all cloudiness before pouring the solvent off so that all of the ultra-fine particles had more time to settle to the bottom of the glass before removing the IPA. I have left the pictures in showing what isopropanol clouded with fine salvinorin particles looks like to show you what not to do, unfortunately I do not have any photographs showing IPA washes as they should look or I would have included them.
I did not try to recover the salvinorin from the first two 25 ml washes of IPA due to the amount of waxy chlorophyll, but could have done so making the total amount of cleaned salvinorin approach 600 mg. Not bad, considering 250 grams of average potency leaf contains about 2.5 mg per gram of leaf for a total of 625 mg of salvinorin.
Growing crystals isn't always easy or guaranteed to be produced each time, but here are two ways that I have done it. The first two methods were taught to me, the third method I developed myself:
Methods to Salvinorin Crystallization:
1. Crystal formation through the cooling of salvinorin saturated hot solvents: Dissolve as much near pure salvinorin powder as you can into 151 proof Everclear Ethanol Alcohol (25% water) warmed to 130-140 degrees F. and then wait for it to cool to see if crystals appear (191 proof Ethanol containing only 5% water might work better). Sometimes I have to re-heat a vial of Salvinorin and Ethanol several times to at or just below boiling before they might grow when cooling. If they are going to appear they should be there within an hour or two. Each time I re-heat a vial containing salvinorin dissolved into 151 Proof Everclear Alcohol I loose some of the Salvinorin and crystals don't always grow, but they usually show up on the fourth try.
2. Crystalline deposits from solvent evaporation: Dissolving high purity salvinorin into Acetone and allowing the solvent to slowly evaporate at room temperature so that it evaporates very slowly will sometimes produce large crystal formations over a period of a few days to a week, but not always. I have grown crystals by evaporating Acetone fairly quickly in either an oven at 120 degrees f (just an ounce of solvent) or by having a fan blow air across an ounce of salvinorin saturated Acetone, but the crystals usually do not form as large as they do when the evaporation occurs slowly. Also, if you have not removed enough of the chlorophyll waxes the crystals will be hard to see, so try to remove as much of it as you reasonably can if your going to try to grow crystals. The extract should be better than 90-95% free of waxy impurities if trying to grow crystals otherwise the waxy lipid fats will hide them from view or stick to the surfaces of the crystalline structures, although if the evaporation container is both small and deep enough like some spice bowls are the dark chlorophyll colored lipid waxes in the solvent usually deposits high up on the sides of the glass as the fluid level evaporates down, by the time the solvent level gets near the bottom of the glass where crystals start to precipitate out of the fluid, most of the Chlorophyll is already out of the solvent.
3. Isolation of crystals from dried extract using Naphtha: Through trial and error extraction research I was surprised to find that the dark waxy extract from a 99% Isopropanol extraction of Salvia divinorum is loaded with small crystals which are formed within the dark waxy compounds as the solvent evaporates. The following explains how to isolate them out of dried extract but will only work if you have removed as much of the tannin contaminate as you can from the extraction solvent first. The way I do this is by letting the extraction solvent sit undisturbed for 12-24 hours to allow enough time for the tannin to settle out of the fluid. Once the tannin has settled pour the extraction fluid into another container for evaporation, leaving the tannin behind. Next, the extraction solvent is completely evaporated leaving a dry waxy extract behind. Once free of any hint of extraction solvent and completely dry, pour in a few ounces of pure Naphtha and scrape every bit of the extract into the Naphtha, including all films which may have formed on the sides of the evaporation container. Completely dissolve every bit of the extract into the fluid until all of the clumps are worked out of it. Once your finished working all of the clumps out of the extract it is very important to leave the container of Naphtha alone to sit still for at least a half hour or more to allow enough time for the fine salvinorin particulates stirred up into the Naphtha to settle to the bottom of the container. After the extraction solids have settled you can then pour the Naphtha off of the extract in the bottom and then add more clean Naphtha back to the container to wash the extract through again, waiting a half hour or more each time. Keep washing the extract with Naphtha until it will no longer take on much more color and has become a light tinted translucent green.
After it's obvious that Naphtha has become ineffective removing additional Chlorophyll and fats and unable to take on more color with each additional wash of the extract, pour off all of the Naphtha and completely dry the extract of any hint of Naphtha. Next, pour in an ounce or more of water into your container of extract and stir for a couple of minutes, allow time for the particles to settle to the bottom of the glass and pour the water off, adding more water to the extract and stirring again. If tannin is present in the extract the water will become a yellow to brown tint, but if using a cup or more of water at a time small amounts of tannin being dissolved out of the extract might be so diluted by that large of an amount of water to be unable to see any change of color to know if its being removed, because of this I like to work with only an ounce of water at a time to be able to know when all of the tannin has been completely removed and I can stop washing with water. Once you are done removing tannin with water completely dry the extract of all moisture and place all of the dried extract into a small two inch diameter spice bowl, or even a small shot glass or something of similar size. Next, pour in enough fresh Naphtha into the glass of extract so that there is about a half inch of Naphtha on top of the extract and briskly stir for about a minute with a spoon, then place the glass or bowl into an electric oven set to about 120 degrees F. with its door cracked open a couple of inches and evaporate all of the Naphtha out of the glass. Keep the small container 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 completely undisturbed in a warm oven while the Naphtha is evaporating off the extract, the heavier salvinorin crystals will all fall to the bottom of the glass while the lighter Chlorophyll impurity forms an upper crust on top. Once all of the Naphtha has been completely evaporated out of your extract you can freeze the glass to cause the top layer of wax to stiffen up enough to be able to easily peel the crust off of the top to expose nothing but golden colored to light green high purity sand-like salvinorin crystals in the bottom of your glass. They might not seem like crystals unless seen under magnification, but they are.
Note: I stumbled upon method three as a complete surprise when I was experimenting with water extractions of leaf for an hour in boiling hot water, then removing the leaf and evaporating the water off all the way down to dry tannin which was then extracted using 99% IPA to recover the salvinorin lost to the water, about 50%. I then removed the tannin from the IPA through settling and after evaporation cleaned the extract with Naphtha as well as I could. After drying the Naphtha cleaned extract I then did a water of the powder just to be sure I had removed all of the tannin contaminates and then after pouring the water off dried the extract. As an added measure, just to make sure the extract was clean enough I added about an ounce of Naphtha to it and stirred the powder into the solvent to see if it would take on any more color, which it didn't, so instead of pouring the Naphtha off I just put it into an oven set to 120 F. to evaporate and was later surprised to find nothing but crystals under a thin crust of dark Chlorophyll colored waxy lipids. These crystals could not have formed within the Naphtha itself because salvinorin is insoluble to Naphtha, so the crystals had to have come strait out of the extract itself, having formed when the 99% Isopropanol was being evaporated down to a dry extract. Prior seeing this, I didn't know that the dark black wax deposited upon evaporation of the extraction solvent had crystals in it and as far as I know neither did anyone else. No one seems to be very interested in using this new method yet, but in my opinion it is the easiest and most efficient way of obtaining high purity crystalline salvinorin that there is.
Warning! The above method of evaporating any amount of Naphtha in an electric oven could cause a fire or worse. I only post this for informational purposes. It worked for me without problems but it might not work for you without causing a fire!
Pictures from method one:
I grew the crystals in the pictures below by dissolving 900 milligrams of refined salvinorin powder (light green color) into 100 ml of hot 140 degree F. 151 proof Everclear drinking Alcohol (Ethanol) and then set aside for two hours at room temperature each time to see if crystals formed. I had to go through three cycles of heating and cooling before these beautiful crystals appeared. The first three times through only a cloud appeared composed of extremely small crystals not visible to the eye except as a cloud. On the fourth heating I came back two hours later and found these beautiful large crystals had formed. When heating your Alcohol thoroughly shake or mix the salvinorin powder into the Alcohol to dissolve as much as possible. Keep adding salvinorin to the hot fluid until I will no longer dissolve any more and has a few specks of solid salvinorin in the bottom which won't completely dissolve to indicate that you have fully saturated the hot Alcohol. When the Ethanol cools back down to 20 degrees C. sometimes salvinorin crystals will precipitate out of the fluid because the Alcohol cannot hold nearly as much salvinorin when cooled down to room temperature. Just leave it alone and let it cool down to room temperature setting on a shelf, nothing special needed. I have used 99% Isopropanol to grow crystals this way too, but they are always much smaller than when using Ethanol. Acetone won't form crystals at all, Methanol will sometimes form larger crystals than Ethanol, but hasn't been as reliable for me compared to 151 Proof Everclear Alcohol which usually takes three or four cycles of re-heating the 100 ml jar before nice crystals form. I have been able to grow crystals in 151 proof Ethanol the same way using a much smaller 30 ml vial of hot Alcohol with as little as 100 mg of Salvinorin producing the same size of crystals.
If you are not skilled using as little 99% IPA as possible to remove all of the lipid or waxy contaminates from the salvinorin extract and or re-work the IPA used to remove the waxy compounds to recover the salvinorin lost to the washes, you can easily loose half of the salvinorin to the Isopropanol washes. Further refinement of the extract through hot solvent saturation and cooling to produce crystals can further increase the losses by half which in the end can easily result in a net of 25% of the salvinorin originally extracted from the leaf! You can recover at least half of the salvinorin lost to the fluid (if you use too much hot Ethanol even more) by evaporating the Ethanol poured off of the crystals, but you will still loose a portion of the yield each time you re-crystallize salvinorin so use as few heating and cooling cycles of the solvent as possible. Re-heating the fluid several times over to produce larger crystals means more loss so use as few heating cycles as necessary and use as little Ethanol as possible too. This can be assured by slowly adding Salvinorin to the hot fluid until you can no longer dissolve any more into it. Once crystals form in the fluid, stop the reheating cycles because they are not purer when larger. If you can see crystals in the fluid, even if you are only able to do so through the aid of a magnifying glass they are pure enough.
These crystals were sent in for analysis and were found to exceed 99.5% purity using HPLC without any other peaks showing.
Pictures from method two
The following two pictures are of some very nice white salvinorin crystals which formed through slow evaporation of Acetone at room temperature. These crystals were produce by adding white salvinorin powder into a small bowl full of Acetone warmed to a temperature of about 130 degrees F. then stirring in as much salvinorin-A powder that could be dissolved into it and setting it aside for a week. When I came back I found these crystals. Sometimes crystals will grow, other times none will form at all. The second picture was taken close up using a zoom stereoscope set to 45X magnification. The light brown colored material at the base of the crystals is tannin sediment that was not removed from the salvinorin powder like I should have.
Pictures from method three:
The following pictures are salvinorin crystals obtained strait out of dried Chlorophyll waxes 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 xhlorophyll 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 photograph on the right was taken with a zoom stereoscope set to 30X magnification.
Can handling pure salvinorin be absorbed through your skin when either dry or when dissolved into extraction solvents?
In my experience Salvinorin in the pure crystalline or powdered form is very safe to handle. I have worked with pure salvinorin both dry and dissolved into various solvents and have never had the slightest effect when handling this compound or solvents containing large amounts of it. Salvinorin isn't easily absorbed through the skin, even when dissolved into Alcohol and held in the mouth salvinorin is poorly absorbed. I have tried using powdered crystalline salvinorin under my tongue from 5 milligrams working in small increments all the way up to 25 milligrams (which is 25 times the amount some individuals smoke) sublingually without Alcohol with absolutely no effect and when swallowed had no effect either. I have also tried up to 25 mg of the powder sublingually together with a few ml of 151 Proof Ethanol drinking Alcohol under my tongue with no effect. It appears that for salvinorin to be absorbed sublingually that it must be thoroughly dissolved into Alcohol or infused into something chewable so that you can thoroughly masticate the powder into extremely fine particles which are small enough to be absorbed, as reported by more than one individual but I have never tried it to know first hand, but I can report that just having pure crystalline salvinorin powder in your mouth with an amount of 151 Proof Ethanol didn't work for me at all. The only caution I can think of is when handling salvinorin is that if you are a smoker and have transferred salvinorin residues on your hands from an extraction onto a cigarette this could cause an unexpected journey, other than that pure salvinorin appears to be almost inert for effect unless absorbed through the use of a properly prepared tincture or smoked.
What are the relative solubility’s of different solvents at room temperature used to extract salvinorin, how much of these solvents does it take to hold an amount of salvinorin?
@27 deg. C.
Acetone: 23 mg per ml. Methyl Alcohol: 3.15 mg per ml (Methanol). Ethyl Alcohol: 1.28 mg per ml. Isopropyl Alcohol: .74 mg per ml.
The green path of Salvia divinorum extractions from black wax to white salvinorin
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!
I just grew a bowl full of beautiful green salvinorin crystals yesterday, the crystals formed all over the bowl, from the top sides all the way down to the bottom. This is the first time I have had crystals forum up high on the side walls of the evaporation container. Interesting that you should mention that right after I saw it for the first time. Goes to show that fluids saturated with salvinorin can grow crystals as soon as it starts to evaporate out, when only a small portion of the solvent has evaporated and thus not due to increased ratios of salvinorin which before I saw this assumed almost forced them to grow. Now I see there is more to it than that.
I will post a picture when I get the time, they are fairly small structures that I have not viewed under magnification yet, but from what I can see they are going to be some of my more interesting crystals to photo document, a fairly dark green color. I took 30 ml of 99% IPA that I used to remove chlorophyll from some old extract that I finally got around to purifying. That first wash took out what looks like more than a 100 mg of salvinorin from the 650 milligrams that I was cleaning but it was done using boiling hot 99% IPA which would cause it to take out lots of salvinorin because I did not wait for it to cool before pouring it off. The second wash took out about 70 mg, but I was only able to recover about 50 mg of it. Where did it go? I have some of it left in the bowl I scraped it out of, but I doubt it amounts to much more than 5 mg, not 20 mg. I will need to wash it out and evaporate it down into a very small container because I can't scrape much more of what is left of the residues using a spoon or knife, I already cleaned that bowl fairly well. I have heard that heating salvinorin in solvents will cause a portion of it to be lost, but if this is true I have no idea where the weight goes or how unless it escapes to the air somehow.
Edit:
Here is a picture of the bowl: 200 mg of green salvinorin crystals which appear a lighter color than they really were due to strong halogen lighting in the left photo, the right photographs color is much better. I only scraped out the green crystals to measure the weight leaving the dark waxes deposited on the upper rim behind which certainly contained some amount of salvinorin too. This in itself is a purification process which can be used too because the chlorophyll impurites always deposit on the upper rim of the evaporation bowl leaving a purer extract below. These crystals were grown by stirring in 650 mg of salvinorin into 30 ml of boiling 99% Isopropanol and then immediately poured off into a small spice bowl which was then placed into a convection oven set to 100 degrees F. for evaporation. On the right is a close up photograph of the round sal xtals.
SWIM thinks that this tek is already all over this forum. The first part seems to be the FAQ that Sphere made a while ago (there might be an updated version).
And the second part more or less seems to be a fused-in version of his actual tek....which can be found in the archive.
...and here is the most updated form of this tek. It's a very good tek that works if done properly.
Hmmm, swim guesses that there are a few questions in the above tek that aren't asked in some places on the forum, so it's worth a read. However, please use the search engine first to avoid posting the same material.
Yeah, I've seen this TEK floating around the 'net back when I was detailing Lizard's extractions.
His opinion is that there is no need for the last step for removing cholrophyll via IPA washes unless one wants to grow crystals for aesthetic reasons. If one has removed the tannins (generally, he'd dissolve the extract one last time in acetone AFTER the Naptha defat to accomplish this), then green crystals ought to be at least 60% pure. Assume 2/3 by weight, and you won't be off by more than +/- 10% in the end product.
Also, re-distill the acetone when possible, because (at the prices Lizard paid), the acetone input is nearly as expensive as the dried leaf! If one lacks distillation capacity, Lizard is of the opinion that the 3rd extraction is counter-productive in terms of cost.
Finally, he feels that, if one could vacuum-filter the "Green crystal" crude sal-a, it would make easier and more efficient than pouring IPA into a shot glass to "wash."
09-04-2008, 16:46
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