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star7896
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Advantages of Soxhlet Extraction
#24172312 - 03/18/17 01:08 PM (7 years, 2 days ago) |
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Hi,
I'm very interested in extractions & am curious about the advantages of Soxhlet extraction. It's a sweet piece of equipment but can anyone who uses one explain what (if anything) is better about this method versus soaking/boiling in ethanol and distilling down to to a smaller volume?
Here's my plan for my first extraction (no Soxhlet):
Crush 120 dried grams down to powder Cover with Everclear and store in a jar in freezer for a couple days Warm up mixture on double boiler Strain solution through grade 90 cheesecloth / squeeze excess ethanol out of mush Filter solution through Buchner funnel under vaccum through grade 1 Whatman filter paper Distill the result down to the smallest volume I can achieve
Given my stated objective, is there any advantage in employing a Soxhlet extractor?
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krypto2000
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Re: Advantages of Soxhlet Extraction [Re: star7896] 1
#24172364 - 03/18/17 01:37 PM (7 years, 2 days ago) |
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I wouldn't use a soxhlet for extracting mushrooms, the alkaloids in mushrooms will be decomposed faster by heat and they readily extract into water and alcohols at RT anyway so there's no need to use a soxhlet. Soxhlets are good for extracting something very, very, thoroughly, say if there's very little of a compound present and you must get all of it, and/or getting hard to extract compounds that a simple solvent soak will not be effective for. There's no real advantage to do it with mushrooms and with heat you have an added disadvantage.
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Bruce Campbell
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Re: Advantages of Soxhlet Extraction [Re: krypto2000]
#24173672 - 03/18/17 11:46 PM (7 years, 1 day ago) |
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I agree with krypto with respect to the mushrooms.
A soxhlet allows for a continuous extraction. You boil your solvent, it rises, hits the condenser, and falls back down (over whatever youre trying to extract from) to the pot. The pot at this point is enriched with your extracted compound. Because the pot is being heated the solvent will boil and evaporate before your desired compound, rise, and repeat the process. This allows for the pot to be enriched more and more and allows for minimal use of solvent.
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star7896
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Great, thanks for the info. So I'll forget about the Soxhlet.
Does everything else look ok with my plan? With 120 grams in a quart of ethanol, is it feasible to get it boiled down to about 1 fluid ounce? Can I expect that it will still be quite fluid at that point? My thinking was the vacuum filtration would be advantageous in this regard. I'm sure it will take some experimentation, just want to know if my expectations are realistic.
Thanks again!
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krypto2000
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Re: Advantages of Soxhlet Extraction [Re: star7896]
#24174328 - 03/19/17 09:50 AM (7 years, 1 day ago) |
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Ime an alcohol extraction will only reduce your weight by 3/4 so you'll still have quite a bit of product left, although it will be much more dense. You can fully dry it out to get a sticky crystaline mass, but it's very hydroscopic so you'll probably need to do so in a vacuum or at least a desiccant chamber.
I don't know how much space 120g powdered would take up, but I'm thinking you'll need to maybe double the amount of ethanol you use, and I would do 2 pulls, so 4qts total. That might be too much, but if you want to be thorough. Also filtering mushrooms is an absolute bitch, it always clogs my filter paper. If you have a fritted funnel than would work better or you could use some celite (can get at a gardening store sold as diatomaceous earth), otherwise expect it to take half a day, it's a real pain. All that goop will clog all of the pores in your filter paper real quick and not let anything else through. Also filtering it hot will definitely improve that.
So I guess what I'm saying is no, you cannot reduce it to 1oz most likely bc the solid material you've extracted will be more than that even, maybe 8oz or so might be more reasonable. If you've got the ability to accurately measure PH and an appropriate organic solvent (DCM, chloroform, ether, something along those lines) then you could do an a/b to get relatively pure psilocin.
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multiporpoise
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Re: Advantages of Soxhlet Extraction *DELETED* [Re: krypto2000]
#24174793 - 03/19/17 01:04 PM (7 years, 1 day ago) |
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Post deleted by multiporpoiseReason for deletion: .
Edited by multiporpoise (03/19/17 01:08 PM)
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krypto2000
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This is the general procedure I've used with success. I've tried it may 3-5 times and have not nailed it down yet though. I've extracted ~5g and gotten a pretty good yield, I'd say at least 80% of the alkaloids recovered. I tried scaling it up though and I yielded the same total amount of alkaloids as I did when extracting 5g though, despite scaling the solvents up too and I'm very confused as to why.
You can substitute DCM or chloroform for the ether which seems to work just fine and vinegar for the GAA (I think they only end up with a 1-2% acetic acid solution anyway). Hydrocarbons/naptha is likely to non-polar to extract the alkaloids. I and another member aschuma have found that using an acidic salt, say mgso4, to dry the solvent does incur a loss though as it converts the alkaloids to a salt so you lose some so you do want to either pick up some sodium salfate or freeze your solvent and then filter off any formed ice. Careful PH control is very important since the alkaloids are sensitive, but otherwise it's a simple extraction and uses readily available chemicals (you may have to order DCM and sodium sulfate online though).
edit: None of those solvents will work except maybe ethyl acetate. Toluene is too non-polar and alcohols and acetone are miscible with water. Ethyl acetate is generally not used for a/b extractions because it hydrolyzes into ethanol and acetic acid in the presence of an acid or a base, but since you're only using a mildly basic solution it would likely be minimal and it is fairly polar for a np so it will probably pull out the alkaloids well.
Aschuma also reported that he found it better to neutralize the acetic acid with a carbonate salt and then basify it with something stronger as he seemed to experience some degradation otherwise, I followed his recommendation, but cannot confirm it's necessary.
Edited by krypto2000 (03/19/17 01:28 PM)
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ichugwindex
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Re: Advantages of Soxhlet Extraction [Re: krypto2000]
#24176622 - 03/20/17 01:20 AM (7 years, 17 hours ago) |
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You guys make me feel dumb as fuck. I wish they let me take chemistry. Ill be lucky to make mushroom gummy bears while the rest of you will be making extractions and shit i could only dream of. I have lots of people asking for doses of mushrooms for ptsd and depression in my country and im just not sure what doses and procedures to use to make a steady easily digested therepy helpful medicine
-------------------- Only hope can give rise to the emotion we call despair. But it is nearly impossible for a man to try to live without hope, so I guess that leaves Man no choice but to walk around with despair as his companion.
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star7896
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Re: Advantages of Soxhlet Extraction [Re: ichugwindex]
#24213182 - 04/02/17 12:45 PM (6 years, 11 months ago) |
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I really appreciate the insight of all in answering my threads on extracts. I'm trying to set up a simple distillation apparatus(distillation flask, liebig condenser, receiving flask) for reducing the volume of my ethanol extract. I'm wondering with this simple setup, and with my stated purpose in mind, if there's much advantage to be had running the setup under vacuum versus just water cooling the condenser... I understand I can boil ethanol at a lower temp under vacuum and perhaps reduce it faster than without the vacuum but does this really make much difference given the relatively low boiling point of ethanol?
Just curious because doing without the vacuum would really simplify my setup, particularly in cold water connections since I would have to run the vacuum off a water aspirator and I will already be wasting water on the condenser.
Any insight would be much appreciated!
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bodhisatta
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Re: Advantages of Soxhlet Extraction [Re: star7896]
#24213205 - 04/02/17 12:54 PM (6 years, 11 months ago) |
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Best way to extract psilocin and psilocybin is boiling water slightly acidulated. Freeze into ice cubes, or add alcohol back in if you want
A soxhlet is 100% useless for what you want to extract
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star7896
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Re: Advantages of Soxhlet Extraction [Re: bodhisatta]
#24213288 - 04/02/17 01:33 PM (6 years, 11 months ago) |
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Perhaps I should have made a new thread - I've already abandoned the Soxhlet based on prior advice. My latest question is on running the distillation setup with/without vacuum...
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bodhisatta
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Re: Advantages of Soxhlet Extraction [Re: star7896]
#24213293 - 04/02/17 01:35 PM (6 years, 11 months ago) |
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Oh well still why use alcohol it's all more soluble in water
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star7896
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Re: Advantages of Soxhlet Extraction [Re: star7896]
#24213298 - 04/02/17 01:38 PM (6 years, 11 months ago) |
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Because I'm curious about it and I want to try it. I'm down with tea, don't get me wrong.
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krypto2000
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Re: Advantages of Soxhlet Extraction [Re: star7896]
#24213343 - 04/02/17 02:00 PM (6 years, 11 months ago) |
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A vacuum will not really help boil it off faster, but it will help in preventing degradation of the alkaloids so I would use it if you have one. It takes the same amount of energy to evaporate a given amount of a liquid regardless what the pressure is, the only time saved is that from heating it to the BP.
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Joshuapsychonaught
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Re: Advantages of Soxhlet Extraction [Re: star7896]
#25032896 - 03/02/18 07:21 AM (6 years, 18 days ago) |
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First off I'd like to bring up the extractor. You use heat making tea so as long as it's only heated as needed and not for an extended period of time such as a 24 hours it should be relatively safe for the goodies. I like to do multiple pulls (4). With the soxhlet you save time and solvent. 4 good pulls can be done in hours without to much hands on work which leaves you open to spills. Handling everything less is usually better. I've lost plenty of stuff to small mistakes such as drops and spills. With reducing the solvent... soxhlet starts near the solvent level you want. I personally use a vacuum distillation kit so I can use less heat and recover my solvent. You can pump run water through the condenser even with an aspirator used for the vacuum. I used a hand pump for brake bleeding to get my vacuum. It even came with a cold collection chamber for the brake fluid or your solvent. Hopefully this helps some one it's my first post.
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