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My salvinorin A Extraction Idea Options
 
Apoc
#1 Posted : 8/25/2011 5:47:50 PM

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Salvia Extraction Method

HI! I thought about this as an idea so that large amounts of solvent don’t have to be extracted. I don’t have much experience with salvia extraction, so please let me know if this idea is not viable.


Step 1: do 3 or more boils of your salvia leaves in nothing but distilled water. Filter out leaves, reduce it down however much you want. Put it in a clear jar or glass. Let sit for a day.

The theorhetical idea here is that since salvinorin is insoluble in water, it should all sink to the bottom, along with all the other impurities. However, the rest of the solution should be all green with plant oils and chlorophyll. This is good because could you not simply suck up most of the water, just leaving the last 10% or so? This would instantly filter out most of the soluble impurities. You won't have to evaporate large amounts acetone.

Step2: Let the remaining water evaporate completely, then re-dissolve it all in some acetone. The insoluble stuff will still sink to the bottom, but most of the salvinorin should be in a solution in that acetone.

You could repeatedly suck up 90% of the acetone, then add new acetone to the insoluble stuff, and suck that up, in order to ensure you get all the salvinorin, while leaving the insolubles behind.

Step 3: Evaporate the acetone

Optional Step 4: In case there is still some impurities in the evaporated acetone, add some water to it and put it in a jar. Add naphtha to the water. They will form 2 separate layers. Shouldn’t the salvinorin sink to the bottom of the jar, as it is insoluble in both water and naphtha? Roll the jar around a bit. The naphtha should pick up some further impurities. Let sit long enough for the salvinorin to sink to the bottom (12 hours).

Step 5: Siphon off the naphtha, repeat adding naphtha as many times as you want. After all the naphtha is siphoned off, evaporate the remaining water.
 

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gibran2
#2 Posted : 8/25/2011 7:15:50 PM

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I’m not quite sure I follow this. Yes, the boiling in water will remove some water-soluble impurities, but water-soluble impurities aren’t really an issue when extracting salvinorin A. Impurities that are soluble in acetone are the problem: fats, oils, other lipids, chlorophyll, etc.

And since you do an acetone extraction in step 2, you’re pulling all of those impurities into solution along with the salvinorin.

So you’re adding a step that really doesn’t seem to do anything.

You’re making salvinorin extraction much more complicated than it really is. I’ve made other posts describing how I do it (using Sphere’s method), but here’s a very quick summary:

--- 1. Add ice cold acetone to salvia leaves.

--- 2. Agitate for 60 seconds, then pour off acetone.

--- 3. Repeat 2 more times.

--- 4. Allow sediment in acetone to settle for 12-24 hours. Decant acetone, discard sediment.

--- 5. Evaporate all acetone in a dark, well-ventilated area.

--- 6. At this point you’ll have a dark green powder that is about one-third salvinorin and two-thirds chlorophyll and other impurities. You can continue to refine it using naphtha and 99% IPA, or use it as-is to make an extract.

That’s it! It’s really very simple.
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jamie
#3 Posted : 8/25/2011 7:24:32 PM

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^would you smoke that stuff though gibran Smile ?..lol..
I made some of that stuff like that that is about 1/3 salvinorin A about 2 years ago..stuck it in a little glass vial and never once had the balls to touch the stuff.

Salvinorin is something I want to purity to xtals..but I just dont know what the hell I would do with it..1mg doses are hard to work with and infuse...I guess I could infuse 20mg at a time into a dropper bottle with ethanol so that each drop is like 500mics..

Sounds frightening the though of accidentally smoking 2mg of salvinorin or something.
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gibran2
#4 Posted : 8/25/2011 7:30:07 PM

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fractal enchantment wrote:
^would you smoke that stuff though gibran Smile ?..lol..
I made some of that stuff like that that is about 1/3 salvinorin A about 2 years ago..stuck it in a little glass vial and never once had the balls to touch the stuff.

Salvinorin is something I want to purity to xtals..but I just dont know what the hell I would do with it..1mg doses are hard to work with and infuse...I guess I could infuse 20mg at a time into a dropper bottle with ethanol so that each drop is like 500mics..

Sounds frightening the though of accidentally smoking 2mg of salvinorin or something.

Oh no – I wouldn’t smoke it. I’d use it to make a more or less “standardized” extract. (I still have my 0.9g of pure salvinorin A I extracted a year ago, and don’t have any specific plans for it.)

I’ve grown about 475g of salvia over the past year, and I’ll probably extract and purify it as I did last year. It’s a lot more convenient for storage, if nothing else.
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Apoc
#5 Posted : 8/25/2011 8:25:48 PM

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gibran2 wrote:
I’m not quite sure I follow this. Yes, the boiling in water will remove some water-soluble impurities, but water-soluble impurities aren’t really an issue when extracting salvinorin A. Impurities that are soluble in acetone are the problem: fats, oils, other lipids, chlorophyll, etc.

And since you do an acetone extraction in step 2, you’re pulling all of those impurities into solution along with the salvinorin.

So you’re adding a step that really doesn’t seem to do anything.


I see, thanks. It's good to know that it would work. You say that the impurities that are soluble in acetone are the problem. But I believe those would also be removed by siphoning off the water tea. The reason I would do this method is so I don't have to buy and evaporate a lot of acetone. It is adding an extra step, but it's an easy step. Simple boils, and discarding the water. From there, you just use the acetone as a solvent, as per usual, except you'd be dealing with a lot less acetone.
 
gibran2
#6 Posted : 8/25/2011 8:43:15 PM

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Apoc wrote:
I see, thanks. It's good to know that it would work. You say that the impurities that are soluble in acetone are the problem. But I believe those would also be removed by siphoning off the water tea. The reason I would do this method is so I don't have to buy and evaporate a lot of acetone. It is adding an extra step, but it's an easy step. Simple boils, and discarding the water. From there, you just use the acetone as a solvent, as per usual, except you'd be dealing with a lot less acetone.

I don't think it will work. And even if it did, you'll still have to use the same amount of acetone - the amount of acetone used is determined by the volume of leaf, not by the nature of impurities present.

Boiling leaves in water will remove some impurities (and for all we know, the salvinorin may be partially bound to some of those impurities, so you might be removing salvinorin as well), but the volume of leaf will be mostly unchanged.

If you want to do this to reduce the amount of acetone used, I don't see how the boiling step helps.
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Apoc
#7 Posted : 8/25/2011 8:48:24 PM

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gibran2 wrote:
I don't think it will work. And even if it did, you'll still have to use the same amount of acetone - the amount of acetone used is determined by the volume of leaf, not by the nature of impurities present.

Boiling leaves in water will remove some impurities (and for all we know, the salvinorin may be partially bound to some of those impurities, so you might be removing salvinorin as well), but the volume of leaf will be mostly unchanged.

If you want to do this to reduce the amount of acetone used, I don't see how the boiling step helps.


I see. I guess the only way to find out is by testing on a small amount of leaf. Smile But no, in this case, I don't think the amount of acetone used would be determined by the volume of the leaf. It would be determined by the volume of sediment that I have after boiling the leaves, and removing the excess water. In the standard tek, the volume of leaf determines the amount of acetone, and I'd rather use less. Your insight is appreciated.
 
gibran2
#8 Posted : 8/27/2011 4:39:38 PM

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After reading post #12 in this thread, I’m thinking you might be on to something. Here’s what I’m thinking:

Although salvinorin A is not soluble in water, brewing salvia leaves may release the salvinorin A from the leaves’ trichomes. If the salvinorin A is kept in solution – not allowed to settle right away – then the tea can be poured off, leaving behind the bulk of the leaves.

Once the tea settles, mainly salvinorin A would settle to the bottom (the grayish precipitate you describe in the other thread?) along with some insoluble plant matter and other debris.

Decanting the liquid and allowing the precipitate to dry would yield – without any acetone – a fairly pure extract. This could be further refined with a small amount of acetone, naphtha, and/or IPA.

Maybe I misunderstood your idea, but I thought you were keeping all of the leaves with the “tea” and allowing it all to dry. If so, then you’re not reducing the amount of plant matter that needs to be processed in subsequent steps. But if you meant that you were pouring off the tea and collecting the sediment from the tea after it settles, then I think you may be on to something.

I have lots of salvia ready for extracting, so maybe I’ll try this with 100g or so!
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Apoc
#9 Posted : 8/27/2011 6:15:12 PM

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Yes, that sums up the idea. A boil should force whatever is in the leaves to come out. Even better, I think freezing the leaves in water before boiling them would further ensure that everything is forced and exploded out of the leaves at a cellular level. Then the water insoluble salvinorin should just sink to the bottom. Filter out the leaves, let the salvinorin settle to the bottom, and siphon off the excess water, and the salvinorin should be at the bottom.

No I didn't have any residue left to save. I don't know why the tea didn't work, and the extract did. If you try the "new" tek, you may want to save the top layer of the tea in case the bottom layer still doesn't yield much. Then you can reduce that and extract from it to still get everything out. As you said, some salvinorin might be suspended in the water. Or, you could still acetone the used leaves, and the discarded (reduced at this point) plant water, to see if it yields anything... just to determine if making a tea really does get all the actives.

The tea looked very clear though, although dark it didn't look like there were any suspensions in it. The tea was so dark though, I don't know if it would be possible to determine the exact level at which the actives have settled. I'd probably just use a thin glass and leave behind the last 10% of the water.

It suppose if the salvinorin is still in water at this point, it would be an option to do the naphtha cleansing first, before acetone dilution, since the water and naphtha will separate. The salvinorin should still sink where gravity tells it to go, the bottom of the jar/glass with the water.
 
gibran2
#10 Posted : 8/29/2011 1:23:20 AM

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OK – I did a test of this idea, and I have good news and bad news.

Good news
Making a tea of salvia leaves and collecting the sediment yields salvinorin A!

Bad news
The yield is about half of what I’d get if using acetone as the initial solvent.



Details

I started with 30g of dried salvia leaf (very fresh – harvested just a few weeks ago). I made a tea using about 300ml of water. I brought the water to a boil with the leaves, then removed it from heat. I let the tea steep for about 10 minutes (same as I’d do with any tea).

I then stirred the mix to make sure the salvinorin (if any) was suspended, and poured the tea out through a sieve.

I did this two more times, ending up with about 1 liter of tea. I didn’t reduce it – I was concerned about what might happen to salvinorin A when heated in aqueous suspension (in crystal form, I think it’s very stable, but I didn’t want to risk destroying it).

I let the tea sit overnight, and noticed that sediment had collected: it was a mix of some leaf particles that passed through the sieve and a finer sediment. I decanted most of the water, then put the sediment plus the remaining water in a smaller container and let it settle again.

When it was settled, I decanted the remaining tea (as much as I could without disturbing the sediment) and then added 50ml acetone to the sediment. I stirred, then allowed it to settle.

After settling, I decanted the acetone and discarded the sediment, which was mostly leaf particles.

I put the acetone in a shallow pan and allowed it to evaporate and the residue to dry thoroughly. I scraped up the residue, and it yielded a light green, sparkly powder – looked just like crude salvinorin A. – That’s the good news.

Now the bad news – I weighed the powder: 68mg.

If this batch of salvia is about as potent as last years (about 2.7mg/g), I should have gotten a yield of over 81mg of pure salvinorin A. The quantity of powder I have is too small to further refine, but my guess is that I got about 40mg salvinorin A. So the bad news is that the yield isn’t nearly as high as it would be when using acetone as the initial solvent.
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Apoc
#11 Posted : 8/29/2011 4:58:53 AM

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hmmmmm, I see. Thank you for trying it. So the good news is it will yield a fairly clean product with hardly any refinement, but only about half the yield as a traditional acetone wash. It is possible your leaves aren't as potent this year, but probably not likely.

Was your product from the water method sticky at all? Or totally powdery? If I can get a non sticky product without even having to use naphtha, I think this still might be worth it for me.
 
gibran2
#12 Posted : 8/29/2011 2:30:32 PM

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Apoc wrote:
hmmmmm, I see. Thank you for trying it. So the good news is it will yield a fairly clean product with hardly any refinement, but only about half the yield as a traditional acetone wash. It is possible your leaves aren't as potent this year, but probably not likely.

Was your product from the water method sticky at all? Or totally powdery? If I can get a non sticky product without even having to use naphtha, I think this still might be worth it for me.

I doubt that the leaves are of significantly lower potency. I haven't done any acetone extractions on them yet, so it's possible, but unlikely.

The extraction result was a non-sticky powder, very similar to the product one gets from a cold acetone extraction, but I'm guessing that the ratio of salvinorin to chlorophyll is higher.

Of course, I took a photo: Smile
gibran2 attached the following image(s):
salvinorin0829.jpg (97kb) downloaded 210 time(s).
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tigerstrike92
#13 Posted : 8/29/2011 4:07:58 PM

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So... even though you didn't get a great yield, that powder/crystals looks freakin awesome.
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Apoc
#14 Posted : 8/29/2011 5:19:47 PM

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thanks for the pic! My acetone extractions have always been very sticky, but it's probably because I let the leaves soak overnight in acetone, and I've also never attempted further cleanup. Do you think that yield is still too powerful to smoke in this form?
 
gibran2
#15 Posted : 8/29/2011 5:46:58 PM

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Apoc wrote:
thanks for the pic! My acetone extractions have always been very sticky, but it's probably because I let the leaves soak overnight in acetone, and I've also never attempted further cleanup. Do you think that yield is still too powerful to smoke in this form?

Never try to smoke a crude extract by itself - it is much too potent. My guess is that this extract is anywhere from 30% to 70% salvinorin A. That's equivalent to 120X to 280X, so a strong dose would be just a few milligrams.
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tigerstrike92
#16 Posted : 8/29/2011 9:08:36 PM

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So if you were going to make a salvia enhanced leaf, would you go this route, dissolve in acetone, and re-vap onto some leaf, or would you go the cold acetone route?
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rOm
#17 Posted : 8/29/2011 9:30:00 PM

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I'd go with ICE-COLD ACE.
This water extract for other application like Apoc suggested.
I've used the ace crude extract onto caapi leaves, it's deliscious !
Smell like tea n,n spirit !

Toke the toke, and walk the walk !
 
Crystalito
#18 Posted : 8/30/2011 12:00:20 AM
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Gibran2 i would like to chime in an idea:

Could you run a small scale experiment where instead of bringing the water to a boil and adding the leafs, you would microwave the water with the leaves inside and then stir it?

Microwaving can improve extraction yields due to destroying cell structures and increasing porosity of the material.

Another idea would be to microwave the leaves first, maybe this method would further rupture the trichomes... You could do a side by side comparison of those 3 (or 2 since you done the first) methods.
 
Apoc
#19 Posted : 8/31/2011 6:12:49 AM

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Crystalito wrote:
Gibran2 i would like to chime in an idea:

Could you run a small scale experiment where instead of bringing the water to a boil and adding the leafs, you would microwave the water with the leaves inside and then stir it?

Microwaving can improve extraction yields due to destroying cell structures and increasing porosity of the material.

Another idea would be to microwave the leaves first, maybe this method would further rupture the trichomes... You could do a side by side comparison of those 3 (or 2 since you done the first) methods.


Why do microwaves destroy cell structures better than boiling? I don't know if I'd trust a microwave to not destroy desirables. Freezing the leaves should destroy cell walls.
 
Crystalito
#20 Posted : 8/31/2011 4:55:20 PM
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Search online for microwave assisted extractions

http://www.sineo.cn/pic/article/42.pdf an example.

Same here , i do not know if it will destroy actives or if it has any advantage hence the proposition for the test. One cannot know until one tries. It goes without saying that one should try it small scale first or on material that wouldnt be too much of a stepback loosing.
 
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