i personally would probably just be more patient with the procedure in general, heating it and getting it to boil violently definitely caused some tar creation and that probably made your product black. I'd probably just air evap the acetone instead. Let the collected acetone from the pulls sit for 24hr or so in the freezer before decanting and removing sediment as well, just to make sure you've got all of it. Then air evap. Maybe warm up the naptha a slight bit above room temp (only maybe like 5 degrees) to increase chlorophyll solubility, and then let it sit for a while (up to 24 hrs probably), keeping it slightly warm if you can. and then decant the naptha (i'd probably pipette it once it gets low to prevent any salvinorin from getting succed with it), and then finish it with isopropyl (using as little as possible since salvinorin is soluble in it). Maybe the iso should be slightly chilled as well to reduce salvinorin solubility. You'll have to do more washings if you do that, but it should reduce the amount of salvinorin it solutes. Some people report only needing 1 minute per pull of acetone, so maybe that might be something to do instead of 3 mins per pull. idk though, this should result in some level of a cleaner product. At the very least don't heat the acetone, that's definitely the worst thing you did.
(Not a chemist) Would using a dehumidifier speed up evaporation by drying out the air? What tools do chemists have to speed up evaporation without using heat?
@@bewertsam Dehumidifying the room wouldn't do anything. If you want to increase the rate of evaporation of an organic solvent you can either decrease the pressure by pulling a vacuum on it or increase air flow with a fan.
My dog told me that when performing chilled extractions you need to make sure that the solvent AND the container are chilled. This will give you a much better extraction from the very start. If Spot was doing this they would probably aim for 0 degrees f, or set the container in crushed ice to make sure that everything stayed as low a temp as possible during this step. He believes that this is easily the most important part of this entire process. Spot also noted that they would probably be a bit more patient during the steps following this, and letting everything evaporate naturally.
Yup 100% right. You need to pre-chill everything, even the glassware. This particular extraction works best at dry ice temperatures with a bunch of acetone with the 🍃 bits in a column
WOW! *Finally* A chemistry video I feel qualified to comment on. Having done this extraction numerous times, here's what I recommend: 1. Extract with acetone. Chilled, not chilled, whatever. You get the salvinorin, along with a buttload of unwanted stuff. 2. After evaporating off the acetone, rinse waxy goo with butane. (Obviously, be careful with a highly flammable solvent.) This will pull off wax; now you have sal-a, chlorophyll, and tannins. 3. With this (much reduced) product, re-dissolve in acetone. Leave it somewhere for it to settle overnight. (Sal-a is sensitive to UV light when in acetone, so I suggest somewhere dark.) 4. After 12+ hrs, come back and decant the solution from the settled tannins. I suggest a syringe or similar...maybe eardropper? 5. Allow green solution to evaporate to dryness. You now have sal-a, plus chlorophyll. All other impurities have been eliminated. This is good to use, as is. If you really want a chemically pure product, continue. 6. Crystallization from dissolving the product in the minimum HOT isopropanol. Then cool in the freezer. Salvinorin-a will drop out of solution. Save the precipitate, discard the solution (maybe use for applications where purity is non-critical, as there's plenty of sal-a in it.) Cheers!
If it's sensitive to light, it's sensitive to heat usually. My guess is you get some diels alder from the furan ring plus whatever other fun things you have in the mix. If you really want to chill the acetone, use a dry ice and acetone bath, cool a beaker in it to minus 78 C with some acetone and use that to do your extract. It will give you a lot more time if your technique sucks but you need some decent gloves to keep it from freezing your fingers off.
@Harry Woodman IMHO, the only reason to chill the acetone is if you want a "one step process" to use the extraction. I don't recommend this because you can get the acetone colder than a well-digger's arse and still pull mostly wax and chlorophyll. (As sal-a is pharmacologically at the milligram level, you want to know potency, and you can't this way.) And, if you defat with butane, and remove tannins anyway, minimizing impurities in step one isn't as big a deal. Sure put it in the freezer, but "no heroic measures." I also suggest NOT boiling acetone. Both because of losses, and because of the flammable nature. Placing it in a Pyrex baking dish in a ventilated area and letting a fan blow across it means you won't create an explosive atmosphere. Plus, acetone is volatile enough that this only takes a couple hours, and it's not like you have to "mother" it the whole time...just do whatever in the same room. The last step, removing the chlorophyll, is lossy, and only necessary if you want crystals or as a "chem flex." I got ~40% from this process, but ultimately I just treated the green crystals as "2/3 purity" and never heard one complaint about strength! (Of course, all this was back in 2008, when this was 100% legal where I lived.)
Yea but it'll never crystalize thst way you could do an a,b on it then try the first step bit the dry ice just do it with water and a pH meter and you'll see ...what happen ...it a guarded secret Hoffman used ....
I really like the advice you guys are giving me! Keep it coming. I do agree, boiling the acetone most likely is the biggest mistake of everything. I guess I have to practice something called patience... The main reason I did it this way was to see if I could speed up the process but alas it doesn't help at all!
Also, even though you did 3 separate pulls, it was all on the same batch of plant material. There was still a lot of acetone in contact with the plant material in between the pulls (causing unwanted material to continue dissolving into the acetone coating the plant material). When you add more acetone to the same batch of plant material, that extra "gunk" was just diluted into the rest of the solution (and then concentrated when evaporated). Given that most of the salvinorin A is found in the trichomes on the exterior of the plant, you only need a small amount of time to dissolve the compound. I would recommend doing a single extraction using significantly more acetone. This way, the trichomes will dissolve faster in the first (and only) pull.
So maybe a 5 minute pull using 2-3 times the acetone would yield cleaner results? I have never done this extraction before, but have a lot of experience extracting THC from weed. You get a LOT more chlorophyll when doing multiple pulls with the same material, for a very small gain in the THC yield. Given that the structure of the plant and location of the active desired compound, is fairly similar to weed, i would highly recommend trying this advice. AS WELL AS, going with VERY LOW or NO heat to aid the evaporation processes, which has already been said a million times in the comment section it seems.
In total you had your plant material sitting in acetone for over 9 minutes, which is definitely too long. Reduce that time good bit and you should be good. Maybe even a single 3 minute pull with much more acetone would do the trick. Food for thought
First of all, it wouldn't surprise me if papers like these aren't 100% reproducible :) It might also be advantageous to do everything EXACTLY like they did in the paper, just to be sure. I don't know if you have the equipment, but you could try a few TLCs and see if you get any results that way. Just dissolve the extracts in a solvent in which the chlorophyll sludge remains at the bottom (and the product doesn't), then filter over a pad of silica gel. Often times you don't even need to do a proper column and just getting rid of polar/insoluble crap can help a lot with things... try for example mixtures of ethyl acetate, THF, acetone, isopropanol or ether in naphtha or hexanes as an eluent
@@chemdelic I love this channel, I need to pay more attention to chemistry so I can become comfortable doing it and make my own psychs, lysergic acid does wonders for my depression. Maybe instead of boiling the acetone, place it under vacuum, I think the heat does something to salvia
@@SilentRacer911 Do NOT, under any circumstances whatsoever, ingest any drug you make in your own basement. You will either kill yourself quick or you will kill yourself slow, either way you will kill yourself if you don't have expert knowledge of pharmaceutical chemistry. If you wanna do drugs just buy your shit off the street and don't make excuses like it helps your depression, there are better drugs to treat depression if that is your issue.
For what it's worth, salvia is no joke. When I tried it, a rift opened up in spacetime in front of me, and I was soon astride two universes, one red and one blue. The trip was hard and I probably won't do it again, but it was also very worthwhile and educational.
I agree with your conclusion from my experience. Reconstructing the concept of time and your reasons for doing what you do from scratch when you come back offers a perspective you can't get without something like salvia.
Do the same procedure as listed but add this to your recipe -patience- you have to let everything evaporate correctly. Heating your flask even at 130 F causes enzymes and other funk to burn. Indirect heat might help but the procedure your taking will work if you do it right. You can also clean it up with heptane since its the same non polar solvent as naphtha is, just let it evaporate instead of burning it. That should help with your crystallization at the end.
Ye this is actually a good point -It should not pull any/much of the chlorophyl which should help you with the colour. Heptane is also 'kinda' low toxicity so u should be good to consume whatever u extract if that's what your going for.
My theory is that the acetone wasn't cold enough. I think placing the extraction flask on some dry ice. Then have the acetone chilled in the same cooler as the dry ice. This should add extra frostivity to the extraction. For a longer duration as well. My background in chemistry consists of youtube, but I have done salvia.
This might help, at the same time tho it seems 0°F is all that's needed. Going colder will only make it take longer, not necessarily increase efficiency of the extraction all together.
I'd distill the acetone first too. I've distilled hardware store acetone from a freshly opened can and had a surprising amount of gunk left behind. Since the finished product is a slight residue in the first place, you want to start with a clean solvent.
Old science rule: the first time when you repeat someone's protocol, you repeat it to the letter, without any changes, then after seeing how it works you start to make modifications. Otherwise it is fudging around in hope that stuff will work
Some notes: - Salvinorin A is very sensitive at least to UV light. So, you should cover the liquids with foil. - Several published extractions do not use heat when drying. - Naphtha may not be good option. I think it will actually dissolve salvinorin A. - Adding drop of acetic acid may increase the stability of the salvinorin A (basic conditions open the lactone ring more easily). Try this way: 1. As before start with acetone (maybe with drop of acetic acid). Filter and dry it without heat. 2. Dissolve to cold methanol. Filter and recrystallize. Edit: Methanol, because it will not dissolve chlorophyll very well and it is suitable for the recrystallization. You might need to do the recrystallization couple times.
OMG! I feel for you. I was one of the first few people to extract salvinorin A (actually, I was the third. I was proceeded by Ortega and Valdes). That was way back in the early 90s. I definitely was the first to ingest pure salvinorin A. Be careful with that stuff. It is extremely potent. Half a milligram is a very strong dose, when vaporized. I don’t have time to step you through extraction procedures. There are a few good methods. The cold acetone method works, but you have to work quickly to minimize extraction of chlorophylls etc. Salvinorin A is excreted by microscopic resin glands on the lower leaf surface. It comes off quickly with a suitable solvent. Cold (freezer cold) acetone washes it off quickly. I’d vacuum filter it off after just 30-40 seconds immersion.. Just work with that first clean pull. You can try to recover more with additional pulls later, but the extracts won’t be as clean.
Boiling the acetone definitely got things hot enough to do weird polymerizations. I think a better procedure would be to powder the leaf, put it in a glass funnel with a filter paper, and then over the course of 10-15 minutes, drip freezing cold acetone over it. Just fill up a sep funnel or addition funnel with acetone, put in the freezer, and do that the day before your procedure. Dry ice is probably unnecessary. The regimen of washing steps seems perfectly adequate, all I would change is the described extraction method with colder acetone and no boiling off the acetone. Don't even use any heat to evaporate things until you're well past the first couple naphtha washes and a water wash, use p a t i e n c e for solvent removal and go gung-ho on the filtering Shouting out this channel would be nice, some subscribers would be a real motivation to get the couple of videos I have edited and uploaded
Allegedly, salvinorin accumulates on the outside of the leaves so powdering shouldn't be necessary and would theoretically (if true) cause more chlorophyll, oils, peptides, etc to be soluted. I'm not sure if this is true. It's definitely true in the case of another psychoactive plant (Cannabis), but i've never used or worked with Salvia so I wouldn't know. It's definitely something to look into though.
you can crush the leaf with a stir bar in dry ice acetone bath, best chill the acetone first, check with a thermometer that handles heavy minus temps and have the natural substrate turning in the flask in the dry ice acetone bath. That will freeze the leaf and help powder it, works best in liquid nitrogen and a mortar and pistil but thats out of your guys league. Evaporation of solvents under vacuum can allow you to remove solvents at negative temperature, again, probably more technique than most can handle but easily done for those that want to learn. Rotovaps are the most common instrument for doing that and they can be equipped with a number of baths and cooling devices that allow all sorts of tricks. My suggestion, take a couple of lab courses at your local JC
I was a cannabis extraction technician for several years for a Licensed Produced up here in Canada, I'm not a chemist but I have a decent amount of experience extracting active compounds from plant matter, I have some really useful tips for how to improvement the process. I think in general your summery at the end is on the right track, however I'd like to really drive the point home that heat is your enemy, it is the devil. Avoid heat at all costs from the very start of the process, there are a ton of very soluble compounds in plant matter which will happily turn to tar if warmed up. Ideally your acetone will be much much colder than 0c, and the solution will stay somewhat cold throughout the entire process. If you can manage it, somewhere around -10c is the warmest I'd go personally for the first step, it can warm up a bit afterword but I wouldn't push it. If 0c is the best you can do, then make sure the entire extraction step takes place at that temperature such as in an ice bath, but I can all but guarantee you'll still end up with byproducts at that temperature. The extraction step can also be improved with the use of a "sock", this is how THC is extracted with ethanol on an industrial scale. Instead of immersing the plant material directly in solvent, the dry material is placed inside a cotton sack that resembles a sock, it's then tied up and submerged in the cold solvent for long time while the solvent is continuously stirred. Never squeeze the sock, to improve yield you unfortunately just have to leave it for longer or do continuous washes. Evaporating the solvent shouldn't be done with heat, it can be done with a vacuum evaporator or very slowly by air at ambient temperature. Some rules of thumb: 1. The colder your initial extraction step, the more pure the product and the more flexible you can be with temperature on subsequent steps 2. Find ways to reduce pouring and filtering, it reduces yield and doesn't work great for these types of processes in general There's far to much info to go over here, but I'd be happy to talk about my experience more if you'd like to send me a DM or something, that goes for anyone in the comments actually. If you want to pick my brain on cannabis extraction hmu, I focused more on solventless extractions, but got to work with the eth process a bit.
I smoked very strong salvia once. It was not pleasant but of course doesn't last long. A few years later I found the bag and wondered why I disliked it so much, and smoked some more. Mystery was solved pretty quickly as I sank to the floor and waited it out.
The weirdest thing about biochem lab was how little lab equipment we ever used. I don't think we ever used a hotplate. One thing you could try if you have access to one is to use a centrifuge for the settling steps.
swim used to be an active psychonaut from 2007-2012 (psy/dis) with sage being the most used and the most sacred, and this has been extremely interesting because this was wondered about prior about extracting the Salvinorin A crystals but found it quite hard to do so. this mimics the same things experienced with messing about with 2c-i/2c-e. subbed
I once messed up a DMT extraction, which I had done plenty of times before with no issue, and I believe it was from trying to concentrate the acidified bark extract by boiling off some of the water on the stove, which I had never done before. Ended up with no precipitate after naphtha extraction and chilling. As others have stated, the high heat and concentration of so many compounds must be inducing some kind of reaction that is destroying the salvinorin.
That scraping step could be avoided very nicely with a sonic bath. I love sonic baths, they help break up clumps of insoluble stuff to help with washes, one would also make short work of any stuck material on glasswear like you have. There's something very satisfying about watching solids fizz around and get decimated under sonication. edit: You might have benefited from focusing on the winterisation (fat/lipid removal) step a bit more by using dry ice. Dry Ice in acetone makes a brilliantly cold liquid. If you're concerned about the slight pH rise from having CO2 in your acetone, you can sit your beaker of acetone in a larger beaker of acetone with dry ice in it. This would absolutely reduce any plant lipids from being dissolved. As for the dark colour that you were remained with, it certainly seemed to have a green tinge to it, indicating chlorophyl, but then you were getting clear naptha washes. It could be that you had some plant cells lingering that were only giving up the chlorophyl a little with each step you did. This may be down to the porosity of your filter paper. For me, if I can, I'll always go with vacuum filtration using something like a 0.45micron nylon filter, or even a 0.2, since you have a vacuum then anything in solution will for sure get pulled right through such filters. Maybe you'd need to play around with the material of the filter with a solvent such a naptha, it's a bit of a wild card naptha I find. There's a wide range of these disc filters that sit on top of a sinter. I hate using the sinters that have fixed walls, I much prefer the ones where you clamp the walls on to the flat sinter. There's a lot less leakage around the edges as well, since the clamped glasswear goes over the edges of the filter disc, stopping anything from going round the edges. Search for "Supelco Mobile Phase Filtration Apparatus 2" to see the type of thing I mean if my description is a bit shit. As for wanting to speed up evaporation, but not use any heat, you can get vacuum chambers pretty cheap, that would absolutely pull off all solvents real nice. You can get pots also that you put under vacuum, seal them closed, then put the whole thing in an oven at 40c, which would make short work of anything residual, even water won't last long at 40c under vacuum, probably best to put a desiccant in there as well if you're vacuum drying to pull off water, phosphorous pentoxide is the champion at grabbing hold of water under a sealed vacuum. I don't actually have any idea why you ended up with such a dark, clumpy, crystal-less mess, but for sure some of the things I've suggested would neaten up a lot of your procedures.
OK chill the acetone on dry ice then extract into a well insulated column packed with Salvia. The extraction must be quick because salvinorin is on the leaf surface only. It should be very pale green. Distill the acetone then dissolve what is left in 10% isopropyl alcohol and water with heat till the alcohol is gone. This will remove the impurities, save the precipitate. This can be purified further with chromatography if desired. Use silica packing and 3:1 chloroform to methanol.
When I make coffee, I filter it through 3 sheets of kitchen towel, because otherwise I get fine coffee particles in my drink. Mby you need a finer filter and other things are passing through the filter you're currently using?
i'd try doing this in a dark flask (as i read that light and high temps could decrease salvinorum A's solubility), as well as using activated charcoal in the acetone solution where u dissolved stuff from the leaves until green color goes away, as chlorophyll could be removed that way. also chill the acetone solution once you've finished extracting from the leaves and are about to filter, i think it'd decrease solubility of contaminants and cause them to settle out. maybe the acetone should be chilled to in the freezer coz 0F (maybe safety concern?). then i'd go about the rest of the procedure as you have here. just some suggestions i thought i'd give though i dont have any qualifications to give them :)
Salvia divinorum can be used as an hallucinogen, Salvia officinalis is sage and can be used insoups and stews, avoid unpleasant confusions while buying .
Try this procedure: Grind the leaves into a fine powder using a mortar and pestle. Weigh out the desired amount of Salvia divinorum powder. Add the powder to a round-bottom flask and cover it with a mixture of acetone and water (for example, 50:50 acetone-water). Heat the mixture to reflux for several hours. This will help to extract salvinorin A from the plant material. Cool the mixture and filter out the plant material. Add hydrochloric acid to the filtered solution to form a salt of salvinorin A. Extract the salvinorin A salt using a non-polar solvent such as chloroform or dichloromethane. Evaporate the non-polar solvent to obtain a crude extract of salvinorin A. Purify the crude extract using column chromatography or another appropriate purification technique. Analyze the purified extract using analytical techniques such as HPLC to determine its purity and concentration.
You can't use a traditional acid-base extraction for salvinorin, because it doesn't contain any ionizable functional groups (i.e., it won't form a salt.) It's actually really unique (as a pshycoactive compund), as it doesn't contain any nitrogen at all (C23 H28 O8). A-B extractions are the gold standard for most organic extractions, but not gonna help here.
its funny because just two days ago i tried salvia for the first time, and just last night had my first major experience. very interesting coincidence.
You want a soxhlet extractor to get everything out. Distilling is the best way to go. I did make hash oil once with naphtha. Just used leave matter with THC crystals on it. Did get to keep the naphtha once i distilled it. Kept it so that there was enough liquid in the flask, and poured that on a flat Pyrex glass oven dish. Once it evaporated, I could scrape all the oil off. Just let it dry enough to make sure that every last bit of solvent is evaporated. Good results, gave a very strong high. :D If everything dissolves in naphtha, use that, because its the cheapest. Do as I described, and use the stuff, either smoke it, or throw it in a cake or something. You should be fine. By the way, I did some research, and when you use pure alcohol (ethanol), you can do an opium extraction on poppy plant material. Just used the steps as ive described before. Greetings, Jeff
My procedure would be: 200g salvia leaves were dried overnight on 40 C and finely crushed to a powder before being extracted with acetone 3 times. The combined extracts were then filtered before the acetone was removed by evaporation under reduced pressure while keeping the extract at room temperature. The resulting crude was then added added ethyl acetate and hexane in a 55/45 mixture until everything dissolved. A column with activated charcoal was prepared to remove any hydrophobic non polar impurities. The column of sand, activated charcoal, sand was added the crude mixture and eluted with ethyl acetate and hexane mixture. The collected eluent was then evaporated to dryness under reduced pressure and the residue was recrystallized from methanol. Careful with the hexane it is carcenogenic.
a few thoughts come to mind. 1. a prewash of the initial material to removed dust/dirt/debris, probably just with distilled water and then allow to thoroughly dry. 2. get your acetone as cold as possible and possibly try reducing the acetone soak to just 2 minutes but do an extra soak or two as this may reduce the chlorophyll that comes across . 3. Avoid excess heat, use a rotovap at low heat or large flat pyrex dish with direct airflow over it to evaporate the acetone and dry the extraction. 4. you could try using an actual filter media on the naptha solution to trap the salvinorin a, and then rinse the media with isopropyl to free the salvinorin a from the media and then rotovap / evaporate off the solvent. 5. check your acetone and naphtha for contaminants. you may need to distill your acetone and if you cant find a clean naphtha, you may want to pick an alternate solvent for this step. naphtha in general can be pretty inconsistent. I also think naphtha may be a bit redundant with your use of Iso propyl as well since both are pretty highly polar compounds and isopropyl is generally much "cleaner". I know in the hydrocarbon extraction of cannabis, processors will do multiple distillations of their butane/propane as most does have greases or lubricants. the only major contaminant in isopropyl should just be water.
When I make weed edibles first I put all the sugar leafs in a container and cover them with distilled water and let it sit a week then slowly pour out the water and put fresh water in for another weak then dry it out and cook it up in butter the water turns green and removes the chlorophyll. Pre soaking the plant matter will get rid of the green chlorophyll and it makes it a cleaner extraction. I think if you pre soak and clean up the leafs first along with the other suggestions it will work.
For extractions like this, I like to add in a dewaxing step then filter through carbon to grab the chlorophyll. Dewaxing is as easy as freezing the extract solution and cold filtering
this channel is fire! finally, it's like nilered turned "educational"! the comedy aspect is a bit wonky, but maybe it's you... it's great tho, love this stuff, btw the majority thinks you are too impatient with all the stuff... if i had to do it maybe make a freezing bath for the acetone or use a peltier to keep it cool, for the evaporation maybe cold + vacuum could help but wtf do i know i'm a mechanic...
Do you think something like a butane extraction could have helped, something less polar. I know when I was younger and did critical fluid exactions with polar and non polar solvents My polar solvent (IPA) final product would end up turning into something like that and when I would do a butane extraction I would age and get crystalline structures. I'm an idiot tho so you tell me.
1. -18c acetone 2. Evaporate the acetone by placing the vessel in boiling water rather than directly on heat. Those are my best guesses. Also, an increase in the amount of starting product may make success easier to see as well as mitigating the negative effect from spilling shit everywhere.
I think you were mostly on the right track. The only extract paper I could find lists the procedure as: "The working amount of 224 grams of dried leaves was crushed to a size of about 1 mm and subjected to extraction three times with acetone. Consecutive extracts were combined. Solid residue was removed by filtration and the filtrate was evaporated to dryness. After dissolution in a mixture of ethyl-heptane acetate (volume ratio 50:40), the solution was passed through a layer of activated carbon to remove coloured components. The solution was evaporated to dryness, and the residue was recrystallized three times from methanol. After the final recrystallization the residue was dissolved in methanol."
The 3 washes part is good. Filter out the solids. Do not heat off the acetone, use a fan over the beaker to evaporate. Use naphtha to remove the tar from the glass and transfer it to a graduated cylinder. Double or tripple the amount of naphtha , stir and let settle for 24 hours. The more naphtha the easier it will be to see the line between what settled and just the liquid. Shine a flashlight behind cylinder and pipette just the liquid out stopping just above the line that settled. Add more naphtha stir and repeat. Each time you wash with naphtha the solids that settle down and the liquid will get lighter. By the 5th or so wash the solids will be very light. You can keep repeating this step until naphtha is clear after stirring and solids are white. Then remove as much naphtha off top. Spread white wet powder on flat surface and let it air dry out by fan. Naphtha takes alot longer to dry out. Then you can finish with the rinses ypu did at the end. The white crystal you end up with should be it.
Chill the acetone using dry ice and alcohol, cold enough it'll freeze the chlorophyll and don't boil the acetone after the washing, spread it out on a baking sheet or something similar to passively dry.
Start with ice cold ground leaves and ice cold acetone. Or colder. Do your extractions, collecting and doing a vacuum evaporation to prevent heat related breakdowns, reductions... Tar.. The colder your acetone the less contaminants, however the naptha steps are ok but you need time for things to settle out. You can do an A+B extraction quickly like this, but when doing washes.. You need to let the little bits settle or you are washing your product away too! Could use a centrifuge if you have one handy! Last up if things aren't separating out the way you want - run a column. You could skip many steps and forget about the in depth process - extract your goods with the acetone and then run a column with that. Many ways to skin a cat, as the saying goes! Love your video titles by the way. Cheers!
Chlorophyll is insoluble in water. Your target molecule is. The first step would be to wash with ethanol, or some sort of small alcohol, since this will dissociate cell membranes and allow you to separate things as you'd like. Just a small amount. Leave it in. Then add water. Tannic acid is also soluble in water, and it binds to proteins and other stuff in the cell, so you'll be left with a mix of everything except chlorophyll in water. After that, you can add cold acetone. Tannic acid is highly soluble in water, so it'll remain in the water layer. Let me know how it goes. I completely made this up btw. Edit: typos
is there a way to do this without naptha? I may or may not have partaken in DMT before but the end result always tastes and smells like naptha. I know naptha is very oily when it comes to solvents so I would like to use something else instead in hopes of getting a cleaner yield.
Did you hypothetically extract DMT with a very small amount of hot naphtha and crash the crystals out in the freezer? Assuming you don't want the max yield, the first few crystalizations should be very clean with almost no naphtha (decant off the cold naphtha to reuse). If the naphtha is left to evap on its own (in a final pull) it always leaves nasty petroleum distillate byproducts.
Limoline is a better option. If someone you didn't know wanted to get a cleaner DMT. The more jungle you go, people don't crystallize. They do a lime juice, sodium bicarbonate "changa" (heavy "a" as the word is Aussie " ) and mix it an aromatic blend. From what I've seen on RUclips you need vacuum distillation of cannabis/limoline solutions to get clean extracts but worth the thought exercersize.
Were you SURE it was salvia? Like it was uh....tried first? Cuz when I tried to do a similar thing with kratom alkaloids, using isopropyl, I kept getting that tar stuff. Perhaps there's an adulterant or bulking agent added to the salvia?
I'm definitely in the camp of "you shouldn't have heated the acetone". Re-do everything, but this time, let the acetone evaporate naturally. Heating the plant material probably caused some kind of reaction that bound some of the material to the final solution, versus letting it wash off during the cleaning phases. Not a chemist, never done this before, but that's the part that jumped out at me as likely being the issue.
I have been soaking some rocks in vinegar and peroxide solution alternating and changing out the vinegar and peroxide solution. In-between I filter and run it through some coffee filters. More than one actually I run it through 3 because I'm finding out that there's a lot of material in the third coffee filter fine particulates.. maybe you're losing whatever you're looking for in that manner. I've honestly considered adding a forced coffee filter just to see if possibly it catches anymore super fines.
ok so in my teens i used to do it this way, 1 pound of fresh not dried leaves. soak the leaves in about half a bottle of everclear. in a glass jug tapped to not let any light in. place said mixture in a closest for a day or two to keep it out of light. i dont know if this is important or not, but just what i always did. after a day or two i would pour off the liquid onto a baking tray and let it evaporate until it was dry. i would get some color but it did not turn as dark as yours. after it was dry i could scrape the pan and gather my crystals. ..... however. this is powerful stuff. using something mugwart or marshmallow leafe to thin it out is highly suggested. ... i did not know the history of it being used by cultures all around the world. now i am interested in learning how it was traditionally used.
Very similar to an old school THC extraction... From your initial wash you picked up too much chlorophyll and waxes. Take your plant material down to the same temp as the acetone. Run your washes, keeping your temp as low as possible. You should end up with something along the lines of green tea, maybe a little darker. Return the acetone to the freezer for an hour or so and re filter (keeping temp as cold as possible) This should catch the waxes and and other unwanteds. Temperature is key in avoiding chlorophyll and waxes.
Try this method, you should get some white crystals: Freeze acetone and soak leafs with freezed acetone for a minute. Remove acetone and repeat two more times. Place extract in freezer until sediment stops forming (~overnight). Decant or coffee filter into shallow evaporation dish leaving solids behind. Evaporate acetone in a well ventilated area. It is recommended to avoid direct sunlight and direct heat. Some water will be absorbed and a fan can speed evaporation, especially towards the end when mostly water remains. Scrape up green powdery residue and transfer it to a small mason jar. Wash powder with naphtha. Allow time to settle and ensure naphtha is clear before decanting to not lose any product. Repeat until solvent is no longer a deep green (light green is OK). Allow napthata to evaporate. Dissolve green powder in boiling 99% IPA leaving any insoluble matter behind. Use a hot water bath or heat plate to warm the IPA (do not have flames anywhere near solvents). Allow IPA too cool and add two volumes of naphtha. Place cloudy solution in freezer for several days. White xtals will grow over time. Decant green liquid, rinse with Naphtha, dry, and recover xtals. Typical yield is 0.2% to 0.3% (100g of dry leaf will give ~250mg of white powder). Optionally, dissolve product in acetone and evaporate slowly to yield larger crystals. Good luck, Green Rat
On the last of his podcasts/interviews H.Morris mentioned himself struggling with trying to extract salvinorin and make it into crystals during his college years, if I remember right
I've never had salvia but the first time was the most potent and I was living in a cartoon world for a while, then started falling into a void as people lined up to watch from a lighthouse, which eventually turned into a 2d picture on the other side of a box, where my body was integrated into the wall behind me. A door opened in my forehead and a man in a black suit stepped out, turned and said "you need to close the lid to remember," so I tried to close the lid of the box - but my hands were too far outside and I started to repeat "my hands aren't in the box, I can't reach the lid." After an indeterminate amount of time, the "lid" closed and I basically snapped back to reality with barely a memory of the event until like a week later.
i think boiling created a resin. i recommend using an alcohol Soxhlet extraction. You can get pretty brilliant crystalline during evaporation. I have always wanted to experiment with Salvia but it recently became illegal in my province of Ontario.
Ice bath while stirring the raw ingredient. Use a chimney vented forced air circulation evaporation technique for acetone evap, with heat but not exceeding 25*c. Use a hand crank centrifuge to induce separation of sediment. Good use on the vacuum separation for larger particulates. Use a brush for scraping to save urself the annoyance. Mayhe for the naptha wash to increase solubility, heat can be used (but don't overheat)?
I think you should do it like a cannabis extraction, frozen, cured, plant matter. Acetone wash, and evaporate. Then dissolve in ethanol freeze and filter the lipids out. Then crystalize.
Wouldn't actually following the current procedure first be preferential to developing a new one? Can you do the solvent processes in reverse order? Naphtha and water first to extract the undesirable components?
i personally would probably just be more patient with the procedure in general, heating it and getting it to boil violently definitely caused some tar creation and that probably made your product black. I'd probably just air evap the acetone instead. Let the collected acetone from the pulls sit for 24hr or so in the freezer before decanting and removing sediment as well, just to make sure you've got all of it. Then air evap. Maybe warm up the naptha a slight bit above room temp (only maybe like 5 degrees) to increase chlorophyll solubility, and then let it sit for a while (up to 24 hrs probably), keeping it slightly warm if you can. and then decant the naptha (i'd probably pipette it once it gets low to prevent any salvinorin from getting succed with it), and then finish it with isopropyl (using as little as possible since salvinorin is soluble in it). Maybe the iso should be slightly chilled as well to reduce salvinorin solubility. You'll have to do more washings if you do that, but it should reduce the amount of salvinorin it solutes.
Some people report only needing 1 minute per pull of acetone, so maybe that might be something to do instead of 3 mins per pull. idk though, this should result in some level of a cleaner product. At the very least don't heat the acetone, that's definitely the worst thing you did.
(Not a chemist) Would using a dehumidifier speed up evaporation by drying out the air? What tools do chemists have to speed up evaporation without using heat?
I strongly agree with this ^
(Chemical engineer, I design processes)
I was gonna suggest a vacuum chamber to quickly evaporate off the acetone.
@@bewertsam Dehumidifying the room wouldn't do anything. If you want to increase the rate of evaporation of an organic solvent you can either decrease the pressure by pulling a vacuum on it or increase air flow with a fan.
@@mitchellr6819 Probably be better to make a parent comment so Chemdelic sees it or reply to his pinned comment at the top.
I'm still waiting for the DEA to barge in randomly
With all their funding they should be able to afford their own .
The DEA sends the instructions
Not the be buzzkill but it’s technically legal in the us.
their already here and collecting IP addresses, probably have a bot that cross checks your IP with social media... got to love modern times
@@lambiiithenoob2970 Not in all states! haha
My dog told me that when performing chilled extractions you need to make sure that the solvent AND the container are chilled. This will give you a much better extraction from the very start. If Spot was doing this they would probably aim for 0 degrees f, or set the container in crushed ice to make sure that everything stayed as low a temp as possible during this step. He believes that this is easily the most important part of this entire process. Spot also noted that they would probably be a bit more patient during the steps following this, and letting everything evaporate naturally.
SWIM also agrees!
Tell Spot he's a good boy and give hime a bone.
Ice-salt bath can help push the temp below 0*C, or so I'm told.
Yup 100% right. You need to pre-chill everything, even the glassware. This particular extraction works best at dry ice temperatures with a bunch of acetone with the 🍃 bits in a column
@@christopherleubner6633 a Husky that I met was wondering about dry ice in acetone or IPA.
WOW! *Finally* A chemistry video I feel qualified to comment on.
Having done this extraction numerous times, here's what I recommend:
1. Extract with acetone. Chilled, not chilled, whatever. You get the salvinorin, along with a buttload of unwanted stuff.
2. After evaporating off the acetone, rinse waxy goo with butane. (Obviously, be careful with a highly flammable solvent.) This will pull off wax; now you have sal-a, chlorophyll, and tannins.
3. With this (much reduced) product, re-dissolve in acetone. Leave it somewhere for it to settle overnight. (Sal-a is sensitive to UV light when in acetone, so I suggest somewhere dark.)
4. After 12+ hrs, come back and decant the solution from the settled tannins. I suggest a syringe or similar...maybe eardropper?
5. Allow green solution to evaporate to dryness. You now have sal-a, plus chlorophyll. All other impurities have been eliminated. This is good to use, as is. If you really want a chemically pure product, continue.
6. Crystallization from dissolving the product in the minimum HOT isopropanol. Then cool in the freezer. Salvinorin-a will drop out of solution. Save the precipitate, discard the solution (maybe use for applications where purity is non-critical, as there's plenty of sal-a in it.)
Cheers!
Do you heat your acetone in step 2?
If it's sensitive to light, it's sensitive to heat usually. My guess is you get some diels alder from the furan ring plus whatever other fun things you have in the mix. If you really want to chill the acetone, use a dry ice and acetone bath, cool a beaker in it to minus 78 C with some acetone and use that to do your extract. It will give you a lot more time if your technique sucks but you need some decent gloves to keep it from freezing your fingers off.
@Harry Woodman
IMHO, the only reason to chill the acetone is if you want a "one step process" to use the extraction. I don't recommend this because you can get the acetone colder than a well-digger's arse and still pull mostly wax and chlorophyll. (As sal-a is pharmacologically at the milligram level, you want to know potency, and you can't this way.)
And, if you defat with butane, and remove tannins anyway, minimizing impurities in step one isn't as big a deal. Sure put it in the freezer, but "no heroic measures."
I also suggest NOT boiling acetone. Both because of losses, and because of the flammable nature. Placing it in a Pyrex baking dish in a ventilated area and letting a fan blow across it means you won't create an explosive atmosphere. Plus, acetone is volatile enough that this only takes a couple hours, and it's not like you have to "mother" it the whole time...just do whatever in the same room.
The last step, removing the chlorophyll, is lossy, and only necessary if you want crystals or as a "chem flex." I got ~40% from this process, but ultimately I just treated the green crystals as "2/3 purity" and never heard one complaint about strength!
(Of course, all this was back in 2008, when this was 100% legal where I lived.)
i think you could also try neutralizing the tannins with a base before you start
Yea but it'll never crystalize thst way you could do an a,b on it then try the first step bit the dry ice just do it with water and a pH meter and you'll see ...what happen ...it a guarded secret Hoffman used ....
I really like the advice you guys are giving me! Keep it coming. I do agree, boiling the acetone most likely is the biggest mistake of everything. I guess I have to practice something called patience...
The main reason I did it this way was to see if I could speed up the process but alas it doesn't help at all!
Also, even though you did 3 separate pulls, it was all on the same batch of plant material. There was still a lot of acetone in contact with the plant material in between the pulls (causing unwanted material to continue dissolving into the acetone coating the plant material). When you add more acetone to the same batch of plant material, that extra "gunk" was just diluted into the rest of the solution (and then concentrated when evaporated). Given that most of the salvinorin A is found in the trichomes on the exterior of the plant, you only need a small amount of time to dissolve the compound. I would recommend doing a single extraction using significantly more acetone. This way, the trichomes will dissolve faster in the first (and only) pull.
So maybe a 5 minute pull using 2-3 times the acetone would yield cleaner results? I have never done this extraction before, but have a lot of experience extracting THC from weed. You get a LOT more chlorophyll when doing multiple pulls with the same material, for a very small gain in the THC yield. Given that the structure of the plant and location of the active desired compound, is fairly similar to weed, i would highly recommend trying this advice. AS WELL AS, going with VERY LOW or NO heat to aid the evaporation processes, which has already been said a million times in the comment section it seems.
In total you had your plant material sitting in acetone for over 9 minutes, which is definitely too long. Reduce that time good bit and you should be good. Maybe even a single 3 minute pull with much more acetone would do the trick. Food for thought
First of all, it wouldn't surprise me if papers like these aren't 100% reproducible :)
It might also be advantageous to do everything EXACTLY like they did in the paper, just to be sure.
I don't know if you have the equipment, but you could try a few TLCs and see if you get any results that way. Just dissolve the extracts in a solvent in which the chlorophyll sludge remains at the bottom (and the product doesn't), then filter over a pad of silica gel. Often times you don't even need to do a proper column and just getting rid of polar/insoluble crap can help a lot with things... try for example mixtures of ethyl acetate, THF, acetone, isopropanol or ether in naphtha or hexanes as an eluent
You could try washing the initial substrate with naphtha before extracting with acetone to avoid bringing any non polar bits with the acetone
Can’t wait to see the improved procedure! Lovin these vids💯
I want to see the communities knowledge come together!
@@chemdelic as do I!
@@chemdelic I love this channel, I need to pay more attention to chemistry so I can become comfortable doing it and make my own psychs, lysergic acid does wonders for my depression.
Maybe instead of boiling the acetone, place it under vacuum, I think the heat does something to salvia
@@SilentRacer911 Do NOT, under any circumstances whatsoever, ingest any drug you make in your own basement. You will either kill yourself quick or you will kill yourself slow, either way you will kill yourself if you don't have expert knowledge of pharmaceutical chemistry. If you wanna do drugs just buy your shit off the street and don't make excuses like it helps your depression, there are better drugs to treat depression if that is your issue.
@@chemdelic make salvia gum next plz (shouldn't be to hard right?)
For what it's worth, salvia is no joke. When I tried it, a rift opened up in spacetime in front of me, and I was soon astride two universes, one red and one blue. The trip was hard and I probably won't do it again, but it was also very worthwhile and educational.
I seem to recall many extra dimensions opening up, and folding over each other. Of the highly-psychedelic substances, this one is by far my favorite.
I became the Spoon Dragon, Second in command to the King Of All Things.
microdosing will open your mind
How long does that kinda trip last? I've heard salvia only lasts about 10 minutes
I agree with your conclusion from my experience. Reconstructing the concept of time and your reasons for doing what you do from scratch when you come back offers a perspective you can't get without something like salvia.
You weren't ready and the salvia knew it
Do the same procedure as listed but add this to your recipe -patience- you have to let everything evaporate correctly. Heating your flask even at 130 F causes enzymes and other funk to burn. Indirect heat might help but the procedure your taking will work if you do it right. You can also clean it up with heptane since its the same non polar solvent as naphtha is, just let it evaporate instead of burning it. That should help with your crystallization at the end.
Ye this is actually a good point -It should not pull any/much of the chlorophyl which should help you with the colour. Heptane is also 'kinda' low toxicity so u should be good to consume whatever u extract if that's what your going for.
yea i agree. I think the boil attributed to a composite resin.
Patience is ket for growing and for procedures in the lab alike key to many things in life ❤
My theory is that the acetone wasn't cold enough. I think placing the extraction flask on some dry ice. Then have the acetone chilled in the same cooler as the dry ice. This should add extra frostivity to the extraction. For a longer duration as well. My background in chemistry consists of youtube, but I have done salvia.
This might help, at the same time tho it seems 0°F is all that's needed. Going colder will only make it take longer, not necessarily increase efficiency of the extraction all together.
@@albummutation2278 it's at 0°C, that's 32°F
agreed.
I'd distill the acetone first too. I've distilled hardware store acetone from a freshly opened can and had a surprising amount of gunk left behind. Since the finished product is a slight residue in the first place, you want to start with a clean solvent.
Lower temperature reduces solubility.
Old science rule: the first time when you repeat someone's protocol, you repeat it to the letter, without any changes, then after seeing how it works you start to make modifications. Otherwise it is fudging around in hope that stuff will work
Some notes:
- Salvinorin A is very sensitive at least to UV light. So, you should cover the liquids with foil.
- Several published extractions do not use heat when drying.
- Naphtha may not be good option. I think it will actually dissolve salvinorin A.
- Adding drop of acetic acid may increase the stability of the salvinorin A (basic conditions open the lactone ring more easily).
Try this way:
1. As before start with acetone (maybe with drop of acetic acid). Filter and dry it without heat.
2. Dissolve to cold methanol. Filter and recrystallize.
Edit: Methanol, because it will not dissolve chlorophyll very well and it is suitable for the recrystallization. You might need to do the recrystallization couple times.
I learned so many things, such a good teaching moment, best educational videos around.
OMG! I feel for you. I was one of the first few people to extract salvinorin A (actually, I was the third. I was proceeded by Ortega and Valdes). That was way back in the early 90s. I definitely was the first to ingest pure salvinorin A. Be careful with that stuff. It is extremely potent. Half a milligram is a very strong dose, when vaporized. I don’t have time to step you through extraction procedures. There are a few good methods. The cold acetone method works, but you have to work quickly to minimize extraction of chlorophylls etc. Salvinorin A is excreted by microscopic resin glands on the lower leaf surface. It comes off quickly with a suitable solvent. Cold (freezer cold) acetone washes it off quickly. I’d vacuum filter it off after just 30-40 seconds immersion.. Just work with that first clean pull. You can try to recover more with additional pulls later, but the extracts won’t be as clean.
Wow! Que you the real Daniel Siebert?!! Haven't seen any publicación from you in a While. Any recomendation on marina the extracto sublingual?
Salvia had me thinking I was a dragon made of a stack of plastic spoons 17 years ago, when you could buy it at headshops.
You still can in my state
Whoa. I randomly search salvia extraction and this video was uploaded 3 hours ago.
This is THE guy you wanna bring to your party
auto click gotta love and support chem content
Boiling the acetone definitely got things hot enough to do weird polymerizations. I think a better procedure would be to powder the leaf, put it in a glass funnel with a filter paper, and then over the course of 10-15 minutes, drip freezing cold acetone over it. Just fill up a sep funnel or addition funnel with acetone, put in the freezer, and do that the day before your procedure. Dry ice is probably unnecessary. The regimen of washing steps seems perfectly adequate, all I would change is the described extraction method with colder acetone and no boiling off the acetone. Don't even use any heat to evaporate things until you're well past the first couple naphtha washes and a water wash, use p a t i e n c e for solvent removal and go gung-ho on the filtering
Shouting out this channel would be nice, some subscribers would be a real motivation to get the couple of videos I have edited and uploaded
Allegedly, salvinorin accumulates on the outside of the leaves so powdering shouldn't be necessary and would theoretically (if true) cause more chlorophyll, oils, peptides, etc to be soluted. I'm not sure if this is true. It's definitely true in the case of another psychoactive plant (Cannabis), but i've never used or worked with Salvia so I wouldn't know. It's definitely something to look into though.
DONT POWDER THE LEAF!!!!! Salvinorin A is on the OUTSIDE OF THE PLANT.
You really want whole leaves for this extraction
you can crush the leaf with a stir bar in dry ice acetone bath, best chill the acetone first, check with a thermometer that handles heavy minus temps and have the natural substrate turning in the flask in the dry ice acetone bath. That will freeze the leaf and help powder it, works best in liquid nitrogen and a mortar and pistil but thats out of your guys league. Evaporation of solvents under vacuum can allow you to remove solvents at negative temperature, again, probably more technique than most can handle but easily done for those that want to learn. Rotovaps are the most common instrument for doing that and they can be equipped with a number of baths and cooling devices that allow all sorts of tricks. My suggestion, take a couple of lab courses at your local JC
You my god sir, are the reason I believe there's great humans out the. Keep up the fantastic work
I was a cannabis extraction technician for several years for a Licensed Produced up here in Canada, I'm not a chemist but I have a decent amount of experience extracting active compounds from plant matter, I have some really useful tips for how to improvement the process.
I think in general your summery at the end is on the right track, however I'd like to really drive the point home that heat is your enemy, it is the devil. Avoid heat at all costs from the very start of the process, there are a ton of very soluble compounds in plant matter which will happily turn to tar if warmed up. Ideally your acetone will be much much colder than 0c, and the solution will stay somewhat cold throughout the entire process. If you can manage it, somewhere around -10c is the warmest I'd go personally for the first step, it can warm up a bit afterword but I wouldn't push it. If 0c is the best you can do, then make sure the entire extraction step takes place at that temperature such as in an ice bath, but I can all but guarantee you'll still end up with byproducts at that temperature.
The extraction step can also be improved with the use of a "sock", this is how THC is extracted with ethanol on an industrial scale. Instead of immersing the plant material directly in solvent, the dry material is placed inside a cotton sack that resembles a sock, it's then tied up and submerged in the cold solvent for long time while the solvent is continuously stirred. Never squeeze the sock, to improve yield you unfortunately just have to leave it for longer or do continuous washes.
Evaporating the solvent shouldn't be done with heat, it can be done with a vacuum evaporator or very slowly by air at ambient temperature.
Some rules of thumb:
1. The colder your initial extraction step, the more pure the product and the more flexible you can be with temperature on subsequent steps
2. Find ways to reduce pouring and filtering, it reduces yield and doesn't work great for these types of processes in general
There's far to much info to go over here, but I'd be happy to talk about my experience more if you'd like to send me a DM or something, that goes for anyone in the comments actually. If you want to pick my brain on cannabis extraction hmu, I focused more on solventless extractions, but got to work with the eth process a bit.
Super chill your leaf and acetone
I smoked very strong salvia once. It was not pleasant but of course doesn't last long. A few years later I found the bag and wondered why I disliked it so much, and smoked some more. Mystery was solved pretty quickly as I sank to the floor and waited it out.
Love your videos man keep it up
This is how literally half of my extractions go :) HAHA Love these videos man keep up the great work
Now THIS is what I expect from a channel named Chemdelic.
You sound like you have a 128 gb 2.5 inch ssd or optical drive for some reason
@@StolenMemes323 You sound like you said something someone would say for some reason.
@@StolenMemes323 You sound like you have a 2.4/5 GHz PCIe WiFi card for some reason
@@SafetyLucas hmm... perhaps, want 2x4gb of ddr3 laptop ram or a random cpu from 2013? send coords rn.
Amazing chem videos 😂❤
I love this channel ❤️
Next week, cooking with Salvia
The weirdest thing about biochem lab was how little lab equipment we ever used. I don't think we ever used a hotplate. One thing you could try if you have access to one is to use a centrifuge for the settling steps.
i had a feeling a video like this was coming
Taking ochem 2 and biochemistry this semester. Finally a channel with reactions I actually find interesting
This is great content 🤠
swim used to be an active psychonaut from 2007-2012 (psy/dis) with sage being the most used and the most sacred, and this has been extremely interesting because this was wondered about prior about extracting the Salvinorin A crystals but found it quite hard to do so. this mimics the same things experienced with messing about with 2c-i/2c-e. subbed
Channel name finally checks out
I finally gave up on filtering and switched to centrifuging my samples. Got a much cleaner separation with virtually no scrap or cleanup problems.
Quality channel
I once messed up a DMT extraction, which I had done plenty of times before with no issue, and I believe it was from trying to concentrate the acidified bark extract by boiling off some of the water on the stove, which I had never done before. Ended up with no precipitate after naphtha extraction and chilling. As others have stated, the high heat and concentration of so many compounds must be inducing some kind of reaction that is destroying the salvinorin.
That scraping step could be avoided very nicely with a sonic bath. I love sonic baths, they help break up clumps of insoluble stuff to help with washes, one would also make short work of any stuck material on glasswear like you have. There's something very satisfying about watching solids fizz around and get decimated under sonication.
edit: You might have benefited from focusing on the winterisation (fat/lipid removal) step a bit more by using dry ice. Dry Ice in acetone makes a brilliantly cold liquid. If you're concerned about the slight pH rise from having CO2 in your acetone, you can sit your beaker of acetone in a larger beaker of acetone with dry ice in it. This would absolutely reduce any plant lipids from being dissolved.
As for the dark colour that you were remained with, it certainly seemed to have a green tinge to it, indicating chlorophyl, but then you were getting clear naptha washes. It could be that you had some plant cells lingering that were only giving up the chlorophyl a little with each step you did. This may be down to the porosity of your filter paper. For me, if I can, I'll always go with vacuum filtration using something like a 0.45micron nylon filter, or even a 0.2, since you have a vacuum then anything in solution will for sure get pulled right through such filters. Maybe you'd need to play around with the material of the filter with a solvent such a naptha, it's a bit of a wild card naptha I find. There's a wide range of these disc filters that sit on top of a sinter. I hate using the sinters that have fixed walls, I much prefer the ones where you clamp the walls on to the flat sinter. There's a lot less leakage around the edges as well, since the clamped glasswear goes over the edges of the filter disc, stopping anything from going round the edges. Search for "Supelco Mobile Phase Filtration Apparatus 2" to see the type of thing I mean if my description is a bit shit.
As for wanting to speed up evaporation, but not use any heat, you can get vacuum chambers pretty cheap, that would absolutely pull off all solvents real nice. You can get pots also that you put under vacuum, seal them closed, then put the whole thing in an oven at 40c, which would make short work of anything residual, even water won't last long at 40c under vacuum, probably best to put a desiccant in there as well if you're vacuum drying to pull off water, phosphorous pentoxide is the champion at grabbing hold of water under a sealed vacuum.
I don't actually have any idea why you ended up with such a dark, clumpy, crystal-less mess, but for sure some of the things I've suggested would neaten up a lot of your procedures.
i love your videos
Love your breakdown, have any inclination to follow up with your take on mhrb? Pretty please..
OK chill the acetone on dry ice then extract into a well insulated column packed with Salvia. The extraction must be quick because salvinorin is on the leaf surface only. It should be very pale green. Distill the acetone then dissolve what is left in 10% isopropyl alcohol and water with heat till the alcohol is gone. This will remove the impurities, save the precipitate. This can be purified further with chromatography if desired. Use silica packing and 3:1 chloroform to methanol.
You could always try a cold press method, like they use for essential oil production
When I make coffee, I filter it through 3 sheets of kitchen towel, because otherwise I get fine coffee particles in my drink. Mby you need a finer filter and other things are passing through the filter you're currently using?
i'd try doing this in a dark flask (as i read that light and high temps could decrease salvinorum A's solubility), as well as using activated charcoal in the acetone solution where u dissolved stuff from the leaves until green color goes away, as chlorophyll could be removed that way. also chill the acetone solution once you've finished extracting from the leaves and are about to filter, i think it'd decrease solubility of contaminants and cause them to settle out.
maybe the acetone should be chilled to in the freezer coz 0F (maybe safety concern?).
then i'd go about the rest of the procedure as you have here.
just some suggestions i thought i'd give though i dont have any qualifications to give them :)
Salvia divinorum can be used as an hallucinogen, Salvia officinalis is sage and can be used insoups and stews, avoid unpleasant confusions while buying .
Try this procedure: Grind the leaves into a fine powder using a mortar and pestle.
Weigh out the desired amount of Salvia divinorum powder.
Add the powder to a round-bottom flask and cover it with a mixture of acetone and water (for example, 50:50 acetone-water).
Heat the mixture to reflux for several hours. This will help to extract salvinorin A from the plant material.
Cool the mixture and filter out the plant material.
Add hydrochloric acid to the filtered solution to form a salt of salvinorin A.
Extract the salvinorin A salt using a non-polar solvent such as chloroform or dichloromethane.
Evaporate the non-polar solvent to obtain a crude extract of salvinorin A.
Purify the crude extract using column chromatography or another appropriate purification technique.
Analyze the purified extract using analytical techniques such as HPLC to determine its purity and concentration.
Not sure if this is right but theres a lot of big words so im gunna assume it is
@@brianbertram4198 I’m hoping he reads it and gives his opinion on if he thinks this would work
You can't use a traditional acid-base extraction for salvinorin, because it doesn't contain any ionizable functional groups (i.e., it won't form a salt.) It's actually really unique (as a pshycoactive compund), as it doesn't contain any nitrogen at all (C23 H28 O8). A-B extractions are the gold standard for most organic extractions, but not gonna help here.
its funny because just two days ago i tried salvia for the first time, and just last night had my first major experience. very interesting coincidence.
I can only imagine how bad that smelled. Strong enough to make your bong taste like it for weeks.
You want a soxhlet extractor to get everything out.
Distilling is the best way to go.
I did make hash oil once with naphtha. Just used leave matter with THC crystals on it. Did get to keep the naphtha once i distilled it. Kept it so that there was enough liquid in the flask, and poured that on a flat Pyrex glass oven dish. Once it evaporated, I could scrape all the oil off. Just let it dry enough to make sure that every last bit of solvent is evaporated. Good results, gave a very strong high. :D
If everything dissolves in naphtha, use that, because its the cheapest. Do as I described, and use the stuff, either smoke it, or throw it in a cake or something. You should be fine.
By the way, I did some research, and when you use pure alcohol (ethanol), you can do an opium extraction on poppy plant material. Just used the steps as ive described before.
Greetings,
Jeff
My procedure would be:
200g salvia leaves were dried overnight on 40 C and finely crushed to a powder before being extracted with acetone 3 times. The combined extracts were then filtered before the acetone was removed by evaporation under reduced pressure while keeping the extract at room temperature. The resulting crude was then added added ethyl acetate and hexane in a 55/45 mixture until everything dissolved. A column with activated charcoal was prepared to remove any hydrophobic non polar impurities. The column of sand, activated charcoal, sand was added the crude mixture and eluted with ethyl acetate and hexane mixture. The collected eluent was then evaporated to dryness under reduced pressure and the residue was recrystallized from methanol.
Careful with the hexane it is carcenogenic.
Do you have the equipment to run separation columns?
a few thoughts come to mind. 1. a prewash of the initial material to removed dust/dirt/debris, probably just with distilled water and then allow to thoroughly dry. 2. get your acetone as cold as possible and possibly try reducing the acetone soak to just 2 minutes but do an extra soak or two as this may reduce the chlorophyll that comes across . 3. Avoid excess heat, use a rotovap at low heat or large flat pyrex dish with direct airflow over it to evaporate the acetone and dry the extraction. 4. you could try using an actual filter media on the naptha solution to trap the salvinorin a, and then rinse the media with isopropyl to free the salvinorin a from the media and then rotovap / evaporate off the solvent. 5. check your acetone and naphtha for contaminants. you may need to distill your acetone and if you cant find a clean naphtha, you may want to pick an alternate solvent for this step. naphtha in general can be pretty inconsistent. I also think naphtha may be a bit redundant with your use of Iso propyl as well since both are pretty highly polar compounds and isopropyl is generally much "cleaner". I know in the hydrocarbon extraction of cannabis, processors will do multiple distillations of their butane/propane as most does have greases or lubricants. the only major contaminant in isopropyl should just be water.
When I make weed edibles first I put all the sugar leafs in a container and cover them with distilled water and let it sit a week then slowly pour out the water and put fresh water in for another weak then dry it out and cook it up in butter the water turns green and removes the chlorophyll. Pre soaking the plant matter will get rid of the green chlorophyll and it makes it a cleaner extraction. I think if you pre soak and clean up the leafs first along with the other suggestions it will work.
For extractions like this, I like to add in a dewaxing step then filter through carbon to grab the chlorophyll. Dewaxing is as easy as freezing the extract solution and cold filtering
Can you use a center fuse for the particles because you hate waiting to decant
Yesss thank you
this channel is fire! finally, it's like nilered turned "educational"! the comedy aspect is a bit wonky, but maybe it's you... it's great tho, love this stuff, btw the majority thinks you are too impatient with all the stuff... if i had to do it maybe make a freezing bath for the acetone or use a peltier to keep it cool, for the evaporation maybe cold + vacuum could help but wtf do i know i'm a mechanic...
Do you think something like a butane extraction could have helped, something less polar. I know when I was younger and did critical fluid exactions with polar and non polar solvents My polar solvent (IPA) final product would end up turning into something like that and when I would do a butane extraction I would age and get crystalline structures. I'm an idiot tho so you tell me.
I absolutely love this, like nile red but with drugs
All that other stuff would help, but I would go with a quick isocratic flash column plus some decolorizing charcoal to clean it up.
1. -18c acetone
2. Evaporate the acetone by placing the vessel in boiling water rather than directly on heat.
Those are my best guesses. Also, an increase in the amount of starting product may make success easier to see as well as mitigating the negative effect from spilling shit everywhere.
Could I only use naphtha? Doesn't thinner evaporate more cleanly?
Jojos to be continued just earned a sub
I think you were mostly on the right track. The only extract paper I could find lists the procedure as: "The working amount of 224 grams of dried leaves was crushed to a size of about 1 mm and subjected to extraction three times with acetone. Consecutive extracts were combined. Solid residue was removed by filtration and the filtrate was evaporated to dryness. After dissolution in a mixture of ethyl-heptane acetate (volume ratio 50:40), the solution was passed through a layer of activated carbon to remove coloured components. The solution was evaporated to dryness, and the residue was recrystallized three times from methanol. After the final recrystallization the residue was dissolved in methanol."
can you do a lysergic acid extraction or even a full synthesis (asking for a friend ofc)
This is one of those extractions where it having some beforehand make everything go faster.
The 3 washes part is good. Filter out the solids. Do not heat off the acetone, use a fan over the beaker to evaporate. Use naphtha to remove the tar from the glass and transfer it to a graduated cylinder. Double or tripple the amount of naphtha , stir and let settle for 24 hours. The more naphtha the easier it will be to see the line between what settled and just the liquid. Shine a flashlight behind cylinder and pipette just the liquid out stopping just above the line that settled. Add more naphtha stir and repeat. Each time you wash with naphtha the solids that settle down and the liquid will get lighter. By the 5th or so wash the solids will be very light. You can keep repeating this step until naphtha is clear after stirring and solids are white. Then remove as much naphtha off top. Spread white wet powder on flat surface and let it air dry out by fan. Naphtha takes alot longer to dry out. Then you can finish with the rinses ypu did at the end. The white crystal you end up with should be it.
I have a pretty good procedure for this. It’s the one you were following, BEFORE you started “doing your own thing” because you’re impatient.
Your acetone gains some water when opened. Try a mineral spirit for less water soluble stuff. Heptane works really well.
Are you gonna do any Acid Base extracts of some Bark on your second channel?
Chill the acetone using dry ice and alcohol, cold enough it'll freeze the chlorophyll and don't boil the acetone after the washing, spread it out on a baking sheet or something similar to passively dry.
Start with ice cold ground leaves and ice cold acetone. Or colder.
Do your extractions, collecting and doing a vacuum evaporation to prevent heat related breakdowns, reductions... Tar..
The colder your acetone the less contaminants, however the naptha steps are ok but you need time for things to settle out.
You can do an A+B extraction quickly like this, but when doing washes.. You need to let the little bits settle or you are washing your product away too!
Could use a centrifuge if you have one handy!
Last up if things aren't separating out the way you want - run a column.
You could skip many steps and forget about the in depth process - extract your goods with the acetone and then run a column with that.
Many ways to skin a cat, as the saying goes!
Love your video titles by the way.
Cheers!
Chlorophyll is insoluble in water. Your target molecule is.
The first step would be to wash with ethanol, or some sort of small alcohol, since this will dissociate cell membranes and allow you to separate things as you'd like. Just a small amount. Leave it in.
Then add water. Tannic acid is also soluble in water, and it binds to proteins and other stuff in the cell, so you'll be left with a mix of everything except chlorophyll in water.
After that, you can add cold acetone. Tannic acid is highly soluble in water, so it'll remain in the water layer.
Let me know how it goes. I completely made this up btw.
Edit: typos
nice video!
is there a way to do this without naptha? I may or may not have partaken in DMT before but the end result always tastes and smells like naptha. I know naptha is very oily when it comes to solvents so I would like to use something else instead in hopes of getting a cleaner yield.
Did you hypothetically extract DMT with a very small amount of hot naphtha and crash the crystals out in the freezer? Assuming you don't want the max yield, the first few crystalizations should be very clean with almost no naphtha (decant off the cold naphtha to reuse). If the naphtha is left to evap on its own (in a final pull) it always leaves nasty petroleum distillate byproducts.
Limoline is a better option. If someone you didn't know wanted to get a cleaner DMT.
The more jungle you go, people don't crystallize. They do a lime juice, sodium bicarbonate "changa" (heavy "a" as the word is Aussie " ) and mix it an aromatic blend.
From what I've seen on RUclips you need vacuum distillation of cannabis/limoline solutions to get clean extracts but worth the thought exercersize.
Will this work with anhydrous acetone?
Were you SURE it was salvia? Like it was uh....tried first?
Cuz when I tried to do a similar thing with kratom alkaloids, using isopropyl, I kept getting that tar stuff. Perhaps there's an adulterant or bulking agent added to the salvia?
It is pure Salvia. I do know that. I really think it was the boiling step of the acetone.
I'm definitely in the camp of "you shouldn't have heated the acetone". Re-do everything, but this time, let the acetone evaporate naturally. Heating the plant material probably caused some kind of reaction that bound some of the material to the final solution, versus letting it wash off during the cleaning phases.
Not a chemist, never done this before, but that's the part that jumped out at me as likely being the issue.
I have been soaking some rocks in vinegar and peroxide solution alternating and changing out the vinegar and peroxide solution. In-between I filter and run it through some coffee filters. More than one actually I run it through 3 because I'm finding out that there's a lot of material in the third coffee filter fine particulates.. maybe you're losing whatever you're looking for in that manner. I've honestly considered adding a forced coffee filter just to see if possibly it catches anymore super fines.
ok so in my teens i used to do it this way, 1 pound of fresh not dried leaves. soak the leaves in about half a bottle of everclear. in a glass jug tapped to not let any light in. place said mixture in a closest for a day or two to keep it out of light. i dont know if this is important or not, but just what i always did. after a day or two i would pour off the liquid onto a baking tray and let it evaporate until it was dry. i would get some color but it did not turn as dark as yours. after it was dry i could scrape the pan and gather my crystals. ..... however. this is powerful stuff. using something mugwart or marshmallow leafe to thin it out is highly suggested. ... i did not know the history of it being used by cultures all around the world. now i am interested in learning how it was traditionally used.
You use a stir bar because you can and you use a vacuum filter because you have to.
its all about following the procedure to the t, maybe a pipette after sediment settles and cold extract
Very similar to an old school THC extraction...
From your initial wash you picked up too much chlorophyll and waxes.
Take your plant material down to the same temp as the acetone. Run your washes, keeping your temp as low as possible. You should end up with something along the lines of green tea, maybe a little darker. Return the acetone to the freezer for an hour or so and re filter (keeping temp as cold as possible) This should catch the waxes and and other unwanteds.
Temperature is key in avoiding chlorophyll and waxes.
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Can I get a Link for leaves
Try this method, you should get some white crystals:
Freeze acetone and soak leafs with freezed acetone for a minute.
Remove acetone and repeat two more times.
Place extract in freezer until sediment stops forming (~overnight). Decant or coffee filter into shallow evaporation dish leaving solids behind.
Evaporate acetone in a well ventilated area. It is recommended to avoid direct sunlight and direct heat. Some water will be absorbed and a fan can speed evaporation, especially towards the end when mostly water remains. Scrape up green powdery residue and transfer it to a small mason jar.
Wash powder with naphtha. Allow time to settle and ensure naphtha is clear before decanting to not lose any product. Repeat until solvent is no longer a deep green (light green is OK). Allow napthata to evaporate.
Dissolve green powder in boiling 99% IPA leaving any insoluble matter behind. Use a hot water bath or heat plate to warm the IPA (do not have flames anywhere near solvents). Allow IPA too cool and add two volumes of naphtha. Place cloudy solution in freezer for several days. White xtals will grow over time.
Decant green liquid, rinse with Naphtha, dry, and recover xtals. Typical yield is 0.2% to 0.3% (100g of dry leaf will give ~250mg of white powder). Optionally, dissolve product in acetone and evaporate slowly to yield larger crystals.
Good luck,
Green Rat
On the last of his podcasts/interviews H.Morris mentioned himself struggling with trying to extract salvinorin and make it into crystals during his college years, if I remember right
I've never had salvia but the first time was the most potent and I was living in a cartoon world for a while, then started falling into a void as people lined up to watch from a lighthouse, which eventually turned into a 2d picture on the other side of a box, where my body was integrated into the wall behind me. A door opened in my forehead and a man in a black suit stepped out, turned and said "you need to close the lid to remember," so I tried to close the lid of the box - but my hands were too far outside and I started to repeat "my hands aren't in the box, I can't reach the lid." After an indeterminate amount of time, the "lid" closed and I basically snapped back to reality with barely a memory of the event until like a week later.
I heard it is a very WILD experience. Crazy that it is legal in most states!!
Wait u jus said u never had it😂
Is this video's intro song, from the game 'Fate' ? -- The sound brought back SO many early gaming memories.
It is actually from a dude that allows royalty-free music. Check the description!
i think boiling created a resin. i recommend using an alcohol Soxhlet extraction. You can get pretty brilliant crystalline during evaporation. I have always wanted to experiment with Salvia but it recently became illegal in my province of Ontario.
Chill your initial acetone down far colder and chill your leaf material.
It will prevent a lot of the waxes and crap dissolving.
Heres a tip it took me a while to learm, pour it confidently, if you pour it too slowly it sticks to the beaker and spills
Ice bath while stirring the raw ingredient. Use a chimney vented forced air circulation evaporation technique for acetone evap, with heat but not exceeding 25*c. Use a hand crank centrifuge to induce separation of sediment. Good use on the vacuum separation for larger particulates. Use a brush for scraping to save urself the annoyance. Mayhe for the naptha wash to increase solubility, heat can be used (but don't overheat)?
Carbonate your water to bring up the ph?
I think you should do it like a cannabis extraction, frozen, cured, plant matter. Acetone wash, and evaporate. Then dissolve in ethanol freeze and filter the lipids out. Then crystalize.
Me pretending to try and figure out what he did wrong even though I have zero chemistry knowledge and just like being the sketchy kid
this is the most impatient chemist i’ve ever seen
Wouldn't actually following the current procedure first be preferential to developing a new one? Can you do the solvent processes in reverse order? Naphtha and water first to extract the undesirable components?
friend asks if you can maybe film educational video on extraction of dimethyltryptamine from Mimosa hostilis root powder