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Invisiblewhiterasta
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Yet another extraction method
    #3552069 - 12/28/04 12:07 PM (12 years, 27 days ago)

I had an older spawn jar covered in aborts which I used this with good result I would expect better from the fruit.This was done fast and dirty for speed. Ideally several washes of the marc would be used.
1pt. spawn(wbs/oyster flour/alder shavings,creeper strain) was placed in a blender w/16oz white vinegar and blended to slush.

slush filtered through poly quilt batting and squeezed to remove all liquid.liquid filtered through coffee filter.

Add VM&P naptha and defat twice.

Dry aqueous phase to thick tar on a glass baking dish,scrape up and place into a smaller vessel( I got about 1 fat tblspn of tar) add methanol (I used 100ml)and stir well with the tar.

You will see the tar imediatly turn whitish and a solid precipitate form stir until preciptitate is washed and filter.

Reduce methanol to 1/3(30ml~) and place in freezer. White crystals form like fine sand immediatly


and continue for a couple days as the alcohol slowly evaps in the frost free (important!) freezer.When the alcohol is reduced by 10x (3ml) it is decanted and the crystals washed with ice cold MgSO4 dried acetone.
Final product is an off white crystalline powder.

Assay of 25mg yielded pleasent +2~ experience.

Doing this fast(an afternoon) and w/o efficiency yeild was 36mg from a single cake.As I said using more efficient technique(multiple washes)this could be tweeked to greater yeilds.

Side note; the drying(hair dryer) of the vinegar extract is very stinky and will burn your eyes w/o proper ventilation.

I am not sure this belongs in Advanced or not but thought it went with the others on this topic.
Bon Chance!
WR :wexican:


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Edited by whiterasta (12/28/04 12:08 PM)


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Offlinetriptamine
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Re: Yet another extraction method [Re: whiterasta]
    #3552093 - 12/28/04 12:19 PM (12 years, 27 days ago)

This is very interesting. I would love to know the extraction efficiency with your method. Also, did you eat only the crystals, or did you eat some of the "goo" with it?

With ethanol alcohol extractions, the crystals are primarily sugar (glucose). One can get psilocybin crystals by precipitating and removing the sugar crystals and then further evaporating until needle like crystals of psilocybin form. Another way is to extract pure psilocin by extracting into dilute acetic acid and doing a gentle a/b extraction to yield pure psilocin crystals. See tek below:

First, use about 10 ml dilute acetic acid (vinegar is fine, or you can even dilute it - pH 3-4 is ok) for every 1 gram of mushrooms. Extract this by soaking about 1 hour. Heat to ~70 degrees C, but don't go too much higher, or you risk destruction of the enzymes responsible for converting the psilocybin into psilocin. Allow to stand at 70 degrees for about 5 minutes and then quickly cool solution by immersing in a water bath (iced is great). After cooled sufficiently (~30 degrees C), filter through a funnel fitted with a filter paper and a cotton ball on top (or you can use celite if you have some). Be sure to pour your liquid into the cotton ball, as this will result in a faster filtering. Then squeeze the remaining liquids out of the fungus. Set this liquid aside. Take the fungus and add about 5ml/gram of fungus more dilute acetic acid, but only swirl around for a few minutes and refilter and squeeze. Combine the filtered liquids and refilter if a poor quality (like coffee filter) filter was used (this will minimize emulsions). Then add about 5ml (per gram fungus) of chloroform to this acetic acid fungus extract. Best to place this on a magnetic stirrer, but constant stirring with a glass rod will suffice. Slowly, and I mean very slowly, add sodium hydroxide solution to this while constantly monitoring the pH. A good concentration is about 10 grams of NaOH to 20 ml water, but be sure to add drip by drip with fast stirring (as high pH conditions can degrade psilocin). Be careful, as when the pH gets near neutral, it can basify quite fast. The target here is pH of 8 and one should not go too much beyond pH of 9. At this basic pH, the psilocin will migrate into the chloroform layer. after mixing well for about 5 minutes, the chloroform can then be separated. Oh yeah, to prevent an emulsion, don't shake for sure, just mix fast, but without introducing air bubbles. Some emulsion will probably be present and can best be eliminated by first letting the layers settle for ~10 minutes and then pouring through a filter with a cotton ball. This will help separate the emulsion. You can then separate the chloroform from the water layer with a separatory funnel or graduated cylinder and pipette and dry under N2, CO2, or other inert gas (no O2, no water). The chloroform will evaporate and leave a residue of crystals of a whitish/yellow color. These can be recrystalized as in the paper to afford pure (>90% psilocin). This can be stored stabiliy in the refrigerator by making a solution of approximately 1mg psilocin, 1mg ascorbic acid in 0.5ml water. The psilocin is not very soluable in water, but will dissolve in time. If done correctly, achivable yields can be >80%

Triptamine


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Invisiblewhiterasta
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Re: Yet another extraction method [Re: triptamine]
    #3552134 - 12/28/04 12:33 PM (12 years, 27 days ago)

Quote:

This is very interesting. I would love to know the extraction efficiency with your method. Also, did you eat only the crystals, or did you eat some of the "goo" with it?




No goo just cream colored crystals @25mg
I believe I am selectively extracting only psilocybin and taking the psilocin as a loss in exchange for simplicity. Note: all "goo" is pretty much left as precipitate and mother liquor is not too thick at the 3ml decant so crystals were not clumpy when dry and before wash. Post wash clean cream colored dry crystals were formed.@ 36~mg/pint cake figuring yield is hard w/o knowing the Psilo content of the cake. But two good trips from an old spent cake is better than a kick in the head,eh?
WR :wexican:

The methanol is automotive HEET (yellow bottle) filtered through charcoal and dried w/ MgSO4


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Offlinetriptamine
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Re: Yet another extraction method [Re: whiterasta]
    #3556483 - 12/29/04 09:55 AM (12 years, 26 days ago)

Hello Whiterasta,

Do you know what the shape of the crystals were? I am interested in your process, but am somewhat concerned that the end crystals will be largely contaminated with sugar crystals as well. Another question: When dissolving the evaporated vinegar "goo" in methanol, does it all dissolve? I would guess that you do this (extract with vinegar 1st, then methanol) to minimize extraction of fats and nonpolar substances - is this the reason?

I know of another method which results in pure crystals of psilocybin:

1. Extract fungus with methanol and allow to dry to a tar
2. Take up tar in a small volume of water (small as possible to dissolve all tar)
3. Add pure (>95% EtOH) to water to bring alcohol concentration to ~85%)
4. Allow crystals to form overnight
5. Crystals are sugar, through away
6. Allow liquid to sit in refridgerator overnight
7. Again remove crystals (again sugar)
8. Allow liquid to evaporate under dry air to yield clear needle crystals of psilocybin.

Triptamine


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Invisiblewhiterasta
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Re: Yet another extraction method [Re: triptamine]
    #3556999 - 12/29/04 01:01 PM (12 years, 26 days ago)

Quote:

Do you know what the shape of the crystals were? I am interested in your process, but am somewhat concerned that the end crystals will be largely contaminated with sugar crystals as well. Another question: When dissolving the evaporated vinegar "goo" in methanol, does it all dissolve? I would guess that you do this (extract with vinegar 1st, then methanol) to minimize extraction of fats and nonpolar substances - is this the reason?




Xtals were quite small and sandy with no real discernable sweetness.Offwhite-cream colored,tryptamine flavor
I wash the vinegar extract solution with naptha to defat.
When washing with MeOH the 'goo" ~90% remains as an off white solid(where I suspect the sugar to be)which is filtered off this leaves a light yellow solution(as pictured)At decant it still is a light yellow and Xtals while small are relatively clean and only need a single Acetone wash to clean up to offwhite.
Dosage of 25mg was a light +2 so I suspect a relatively pure product.

I did forget a step, during the vinegar phase before defatting I add 500mg ascorbic acid and refilter(hopefuly preventing oxidation during the concentation of the vinegar extract).

the "goo" after the methanol wash is hard, crunchy and easily filtered. It turns white immediatly upon adding the methanol and washes very rapidly to whitish chunks with stirring.
Also note a VERY strong acetic aroma upon evap of vinegar extract(eye burning)almost like a latex paint but far more acetic and irritating,Totally unlike say boiling cucumbers in vinegar for pickles.
Also note this was done with a myc cake so I was extracting whatever substrate also. This needs repeating with just dry fruit to see any differences in the process(I am most curious regarding the methanol wash and resulting precipitate)
Last note this was a moments inspiration not a well thought out protocol, so please forgive the "roughed out" nature of the algorythym.
WR :wexican:


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Offlinetriptamine
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Re: Yet another extraction method [Re: whiterasta]
    #3560510 - 12/30/04 08:07 AM (12 years, 25 days ago)

Sounds good. Let us know how your next experiment works out. Perhaps a TEK next time?

Triptamine


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Offlinejeff01
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Registered: 12/17/04
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Last seen: 12 years, 13 days
Re: Yet another extraction method [Re: triptamine]
    #3563721 - 12/31/04 01:33 AM (12 years, 25 days ago)

good stuff


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