Chilled Acetone Extraction For Salvia Divinorum @ SALVIA-COMMUNITY.net
 

 
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post Jul 17 2004, 09:35
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Crystal Grower


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Note: The rest of this tek is on page two of this thread, after adding more information I ran out of room to put it all in two posts due to text limits.

Reduced Lipid Extractions Using Chilled Acetone

Salvia Divinorum Extractions Using Chilled Acetone. December 30, 2005.
By Christosphere

QUOTE
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.

Bild: http://boards.marihemp.com/boards/research/media/4/4577.jpg

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.

Der Beitrag wurde bearbeitet von Sphere am Dec 31 2005, 12:12 Uhr.
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post Nov 26 2005, 03:39
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Grünschnabel


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where you get your acetone? 22€/L isnt cheap i guess..
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post Dec 3 2005, 17:57
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Salvia Kenner
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I don't know what's the problem with Acetone? Of course it's flammable but it is much safer to work with it in comparsion with CHCl3 (don't know if the english word is the same as the german one) or anything similar.

We use Acetone for cleaning (glassware, our hands,...) because it's safe to handle.

I'm sorry for my bad english smile.gif


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Wer nicht auf seine Weise denkt, denkt überhaupt nicht. (Oscar Wilde)

Denken ist eine Anstrengung. Glauben ein Komfort. (Ludwig Marcuse)
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post Jan 1 2006, 16:26
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Crystal Grower


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QUOTE(Prometheus @ Dec 3 2005, 17:57)
I don't know what's the problem with Acetone? Of course it's flammable but it is much safer to work with it in comparsion with CHCl3 (don't know if the english word is the same as the german one) or anything similar.

We use Acetone for cleaning (glassware, our hands,...) because it's safe to handle.

I'm sorry for my bad english smile.gif
*




Acetone isn't dangerous to work with except for flammability. I put the warnings in the next as a disclaimer only, in case someone isn't careful enough.
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post Jan 26 2006, 12:07
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Crystal Grower


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I recently finished adding photos to my Salvia divinorum Chilled Acetone Extraction tek. You can download it at this URL: http://www.imageevent.com/sphere - 2.2 meg .pdf file.
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