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InvisibleVinci
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Re: Crystals [Re: DINKLB3RG]
    #27340036 - 06/08/21 10:34 AM (2 years, 11 months ago)

Quote:

DINKLB3RG said:
Solvent was the same as described. (wet ethanol)


The ISOLATE won't crystallize if you don't manipulate it. That's correct.

this is a trehalose+active structure. I think this would be classified as an extract not an isolate. (This was done with nothing but 180 proof)

I've had luck crystallizing out of AB extraction. anyhydrous methanol/ethanol work for ReX

The Isolate crystals are translucent and needle like.

also just read something on an 80/20 acetone mix with water. if anything I feel like that would clean it up the most. allowing the sugars to stay in solution with the water. while actives drop out in cold acetone.


also a large portion of the Hoffman paper. I went out and searched it. describes chromatography methods for isolation. only mentioning halogen preventing the crystalization.

if you need an isolate the chances are you're going to try vaping it. I would fill a cart and not need a crystalline isolate.


science does update from time to time. solvent rated membranes are fun.

Hoffman's experimental:
https://patents.google.com/patent/US3183172A/en

I've also had crystals precip out of the alkanes after preforming A/B on extract. however I recommend finding a better NP solvent for your pulls and then use the tane to clean up

I want to try a couple things for further clean up.
I would like to try sublimination as well as a Straight To Base process. I just haven't gotten around to it yet



Damn! Didn't expect to read this from a new account. Cheers brotha. Is your sig image pans or small cubes on the left?


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Vinci luh you

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OfflineDINKLB3RG
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Re: Crystals [Re: Vinci]
    #27340171 - 06/08/21 12:06 PM (2 years, 11 months ago)

it's a smaller cubensis var. AA+ iso I worked on. it got crazy good flushes.


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OfflineEnDelfisE
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Re: Crystals [Re: DINKLB3RG]
    #27341135 - 06/09/21 05:54 AM (2 years, 11 months ago)

Quote:

DINKLB3RG said:
Solvent was the same as described. (wet ethanol)


The ISOLATE won't crystallize if you don't manipulate it. That's correct.

this is a trehalose+active structure. I think this would be classified as an extract not an isolate. (This was done with nothing but 180 proof)

I've had luck crystallizing out of AB extraction. anyhydrous methanol/ethanol work for ReX

The Isolate crystals are translucent and needle like.

also just read something on an 80/20 acetone mix with water. if anything I feel like that would clean it up the most. allowing the sugars to stay in solution with the water. while actives drop out in cold acetone.


also a large portion of the Hoffman paper. I went out and searched it. describes chromatography methods for isolation. only mentioning halogen preventing the crystalization.

if you need an isolate the chances are you're going to try vaping it. I would fill a cart and not need a crystalline isolate.


science does update from time to time. solvent rated membranes are fun.

Hoffman's experimental:
https://patents.google.com/patent/US3183172A/en

I've also had crystals precip out of the alkanes after preforming A/B on extract. however I recommend finding a better NP solvent for your pulls and then use the tane to clean up

I want to try a couple things for further clean up.
I would like to try sublimination as well as a Straight To Base process. I just haven't gotten around to it yet





This is amazing info! Ive looked long ago into getting the actives down to crystal fork but all I could find was people saying it's inactive starches, so there is a way after! Thank you for sharing brother! Please  be updating us!

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OfflineCyonic
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Re: Crystals [Re: EnDelfisE]
    #27347135 - 06/13/21 06:57 PM (2 years, 10 months ago)

There is a tek for extracting psilocin at thenook

4 hour process if I remember correctly.


Psilocin is soluble in acetic acid. I believe methanol is involved.

Freebase psilocin, (4OH-DMT) Clcan be smoked for nnDMT like experience which shouldn't be too surprising. It's more potent than nnDMT.  Only takes around 40mg for a average sized adult male where as nnDMT is more like 70mg.

Edited by Cyonic (06/13/21 07:04 PM)

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InvisibleVinci
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Re: Crystals [Re: Cyonic]
    #27347908 - 06/14/21 12:37 PM (2 years, 10 months ago)

Link please?


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OfflineCyonic
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Re: Crystals [Re: Vinci]
    #27348643 - 06/15/21 01:19 AM (2 years, 10 months ago)


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OfflineSolipsis
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Re: Crystals [Re: Cyonic]
    #27348837 - 06/15/21 06:52 AM (2 years, 10 months ago)

Yea a typical alcoholic extract might contain small amounts of alkaloids and this is what the "crystals of the gods" people were perhaps excited about cause the tincture might have worked but I can't imagine they did the maths on the precipitate.
I think it is known to contain a bunch of sugars and proteins as impurities.

Still working on it but my plan is to use methanol for the extraction but do it totally anhydrous, and finalize with a solvent purification step but not sure if crystals can be expected. Might also involve artful recrystallization but seems to me what we are talking about avoiding is mostly doing column chromatography which I do recall Hofmann using, the "halogen" stuff aside.

Anyway thanks, will certainly look into the acetic acid thing but are proteins and sugars really not soluble in that, when the acetic acid concentration is high enough? Because aqueous acetic acid is a suitable solvent if you purify it anyway later but that's not what I think we are talking about.

Checking that out further and the claim does look quite nice about the purity but it seems strange to me that it works, I wonder if the sugars are primarily poly- and oligosaccharides and thats why the solubility in chloroform is so poor.

You would need to have the psilocybin converted to psilocin if the chloroform (or i suppose xylene) is to dissolve it but luckily the acid should do that conversion.

If this works like it says it seems preferable over what i had planned.

Edited by Solipsis (06/15/21 07:39 AM)

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OfflineDINKLB3RG
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Re: Crystals [Re: Solipsis]
    #27348974 - 06/15/21 08:57 AM (2 years, 10 months ago)

use of acetic acid aids in the dephosphorylation of the ethanol extract.

you can even wet your etoh with vinegar. as long as your pH is around 4 you'll have total conversion of Psilocybin into Psilocin


acetic acid is usually used as the A in AB, or for salting the final freebase to be bioavailable.

it's nice because when it evaporates it doesn't leave a crystalline solid like citric acid would.

however. it's only an acid to assist with the compounds transferring to the aqueous layer during AB.


also I highly recommend only using ethanol if you're making a food safe product. or if you're attempting to vape

I doubt anyone here has capabilities for residual solvent testing for methanol. just be safe is all.

thought anhydrous methanol doesn't work well like anhydrous ethanol, no?


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OfflineSolipsis
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Re: Crystals [Re: DINKLB3RG]
    #27355197 - 06/19/21 01:08 PM (2 years, 10 months ago)

I've looked at this a couple more times and started planning, it's a quite nice method as a basis. But there are a couple of things I don't understand or might try/change:

- Why not heat with a waterbath during the extractions/pulls but heat it afterwards - only for the filtration? Does extracting hot maybe co-extract the wrong things?
- It seems to be forgotten to be mentioned to include the ascorbic acid in the second pull.
- It's not that the freebase wouldn't be bioavailable (orally that is) since it just gets salted in your stomach and the muriatic acid salt seems fine to me, but it would be considerably less stable, you sometimes see salts like fumarates for synthetic 4-substituted tryptamines. I suppose tartrate should also be pretty good and actually the citrate doesn't seem like a bad idea to me. In this method ascorbic acid is also suggested as a stabilizer, it is unclear if it works so well because the alternative they had was the unstable freebase, or because it is an anti-oxidant, or both... but you do not have to evaporate any excess if you only do it stoichiometrically. Not sure if thats the idea behind the 50 mg and 50 mg, maybe that could be more precise, actually based on molar weight.
- What is (fb) psilocin insoluble in, lol? Cause it would be interesting to do some simple tests on the ascorbic acid combined product, supposedly the ascorbate, would like to see how weak of a base psilocin is (otherwise as a zwitterion, the binding / relationship becomes puzzling to me).
- Don't worry about a drop of residual methanol, look up how many mL you can drink each day without even reaching the toxicity limit - in other words, amounts not even close to what can fit in about 15-30 mg of crystalline product, but far beyond. Be safe but also realize toxicity is a matter of dosage and not a blanket statement about a compound. You need to know what you are doing though, don't stop worrying about it before that but after :wink: Maybe you don't like the idea of ingesting methanol but you can get methanol into your body as a result of eating, drinking and metabolizing random compounds and your body is capable of dealing with a certain amount just fine - same for many other things that would be considered toxins if it would really get out of hand.

I think I wanna add a bit more glassware before I go ahead with this, although a small test quantity not really a reason to wait with that tho i have my chloroform elsewhere. Was thinking about getting some xylene for some reason I forgot already (maybe also cause of red jungle spice), however chloroform is much easier to evap and can actually be distilled over for the most part to recover it, using a waterbath unlike xylene with its high boiling point.
To add the chloroform/xylene, maybe its cool to use a dropper funnel and just put a separatory funnel until a dropper is acquired. A soxhlet seems overkill for this and may actually not be such a good idea, which brings me full circle to question 1.

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OfflineEnjoil
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Re: Crystals [Re: Solipsis]
    #27356193 - 06/20/21 08:51 AM (2 years, 10 months ago)

This seems like a lot a lot of work? Who isn’t happy with just eating a fresh or or making a cup of tea?  Well maybe cuz now mushies are legal in Oakland they will be like weed. All the good weed will disappear and we get oils and goo! Maybe they do the same with the mushrooms?

It seems like an ez dose pill would be good. Has any heard of those pills that are supposedly psilocybin. Idk dude was calling them instant shrooms in Tucson when I was a kid. I think it was some kind of synthetic mescaline or 2cb. Idk that pill was crazy, kicked in within ten minutes and I lost track of everything time stood still and I was thinking I was the one who had to fix it!  I’m totally not qualified for that job, fixing the time space continuum. Ha ha. Well looks like mission accomplished!

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InvisibleVinci
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Re: Crystals [Re: Enjoil] * 1
    #27357409 - 06/21/21 10:41 AM (2 years, 10 months ago)

The cubensis experience is far from a pure psilocin/psilocbin experience. If you eat a pan, you get less mushroom and more psilocybin/psilocin, and the experience is much less body based. I'd say it's a cleaner feeling. This could have to do with other actives (baeocystin, norbaeocytin, aeruginascin, norpsilocin, ß-carbolines) being less present in the pans, or maybe even more.. So I'd say it's very worth exploring the each component of the experience separately.


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OfflineAlan RockefellerM
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Re: Crystals [Re: Vinci] * 1
    #27358203 - 06/21/21 09:18 PM (2 years, 10 months ago)

A friend in Germany made these recently from fruits of Psilocybe cubensis.  The solvent was methanol and HPLC was used for purification.  Crystalized with acetone.


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OfflineEnjoil
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Re: Crystals [Re: Vinci]
    #27358239 - 06/21/21 09:55 PM (2 years, 10 months ago)

Cool. That seems very reasonable.  I have only had a few normal cubes so far. Plenty of em but nothing special. Bi just got a few different exotic types to try and check out. So I’m excited to see what your talking about.

I wish it was as easy to make some psilocybin crystals as it is to stand on a hair straightener and get wax!

I gave my cousin some mushrooms and he told me he smoked them. I was like” I think it’s a different kind of mushrooms people smoke and I think it’s also just the skin or veil of it.

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OfflineDINKLB3RG
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Re: Crystals [Re: Enjoil]
    #27361140 - 06/24/21 06:29 AM (2 years, 10 months ago)

Quote:

Enjoil said:
This seems like a lot a lot of work? Who isn’t happy with just eating a fresh or or making a cup of tea?  Well maybe cuz now mushies are legal in Oakland they will be like weed. All the good weed will disappear and we get oils and goo! Maybe they do the same with the mushrooms?

It seems like an ez dose pill would be good. Has any heard of those pills that are supposedly psilocybin. Idk dude was calling them instant shrooms in Tucson when I was a kid. I think it was some kind of synthetic mescaline or 2cb. Idk that pill was crazy, kicked in within ten minutes and I lost track of everything time stood still and I was thinking I was the one who had to fix it!  I’m totally not qualified for that job, fixing the time space continuum. Ha ha. Well looks like mission accomplished!




you can fit a 3g equivalent dose in a size 0 capsules.

however. you can fit even more of a dose in a gummy.


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Edited by DINKLB3RG (08/03/21 09:02 AM)

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OfflineDINKLB3RG
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Re: Crystals [Re: Alan Rockefeller]
    #27361145 - 06/24/21 06:37 AM (2 years, 10 months ago)

Quote:

Alan Rockefeller said:
A friend in Germany made these recently from fruits of Psilocybe cubensis.  The solvent was methanol and HPLC was used for purification.  Crystalized with acetone.






any insight on filtration media?
I read something about microcrystalline cellulose as the stationary phase


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OfflineDINKLB3RG
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Re: Crystals [Re: Solipsis]
    #27361922 - 06/24/21 07:07 PM (2 years, 10 months ago)

been doing it in a 1l soxhlet. yeah, little over kill and slow run time. takes about 4 hours to have it run clear.

Theres better options im already looking at.


I like to extract HOT then room temp evap. unwanteds precip out


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Edited by DINKLB3RG (06/24/21 07:09 PM)

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OfflineEnjoil
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Re: Crystals [Re: DINKLB3RG]
    #27362358 - 06/25/21 06:02 AM (2 years, 10 months ago)

I thought I read that the crystals need to be kept in some kind of solution so they don’t start degrading.  That would be an awesome gummy bear! 

I made some truffles a few days ago and it a pain in the butt to mix each one individually with a toothpick. I found some espresso flavored chocolate chips and mixed em with normal milk chocolate and they came out delicious.

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OfflineMerryTerry
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Re: Crystals [Re: DINKLB3RG]
    #27365578 - 06/27/21 08:04 PM (2 years, 10 months ago)

Very intrigued... Nice one. Have you heard back from Oakland?  Will you post the results of the sample?


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OfflineShiro
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Re: Crystals [Re: Vinci]
    #27366136 - 06/28/21 11:01 AM (2 years, 10 months ago)

So I got a Soxhlet extractor for this just for most to say that’s overkill. I for one am excited to use it (;


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OfflineShiro
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Re: Crystals [Re: Enjoil]
    #27366137 - 06/28/21 11:02 AM (2 years, 10 months ago)

The crystals oxidize quicker than good L. Yes. So suspension is a must.


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