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OfflineNoOneKnowsHowToAct
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Re: Potency Project [Re: Necco]
    #11816232 - 01/12/10 04:19 PM (15 years, 7 days ago)

Some links I've found while searching. There are some interesting and simple looking techniques in here:

http://www.erowid.org/archive/rhodium/chemistry/psilocin.extraction.html
http://www.cognitiveliberty.org/shulgin/adsarchive/extraction.htm
http://www.erowid.org/plants/mushrooms/mushrooms_journal1.shtml
http://www.lycaeum.org/nepenthes/Extraction/extract5.html
http://deoxy.org/wiki/Mushrooms/Alkaloid_Extraction

I need to get me some actual ammonia. I picked some up from the supermarket even though it said it had a surfactant in it. If it'll still get me SOME crystals I'll try it although I wouldn't use it for any measurement procedure.

Is 2.8 too acidic? Will that not work? I assumed it would be fine since it was below 4. I went with straight vinegar. Some of the other things I had read seemed to indicate that this would be ok and that it wasn't critical that the initial solution have a pH of EXACTLY 4. In theory, I could just evaporate my acetic acid solution right? I'm curious, I have ~ 5lbs of indicating dririte (CaSO4). Would I be able to evaporate extremely quickly using this?

Ideally I'd like to get something that'd keep easily for long periods of time, but it seems that all of the alcohol extractions are not ideal for this since they give you pure psilocin crystals which readily oxidize when exposed to air.

I had not found a good substitute for the diethyl ether. I'm open to suggestions. I'm no chemist either. I was going to simply try using naphtha at that point to see if I come up with anything.


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InvisibleNecco
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Re: Potency Project [Re: NoOneKnowsHowToAct]
    #11816359 - 01/12/10 04:38 PM (15 years, 7 days ago)

Yeah, that is what I'm not sure on. I don't know if a very acidic environment is harmful, all I know is that it isn't necessary. More the reason why I was thinking we should use as little as possible, is so that we don't have to overly dilute the extraction solution with the base.

There is no need to try to evaporate the acetic acid. I'll add that any evaporation step is likely to be very tricky because of the fragility of psilocin. When it comes time to evaporate the non polar, we should do our bests to either distill off the solvent (preferably under reduced pressure) or by evaporating with a stream of "inert" gas.

BTW, it seems like you are assuming that we are going to end up with a phenolate salt in the end. I'm fairly certain that we will have plain psilocin after basing and extracting with the N/P.

Once crystals are obtained, I think that they will keep alright so long as they are stored in amber bottles with as much oxygen evacuated as possible. (or you could put it back in to solution, alcohol, and preserve with vitamin C)

I don't think that naptha will work well. Naptha is essentially hexane, and hexane is used in the recrystallization step because of psilocin's poor solubility in it (this step is described in the link I posted). I perhaps tetrachloroethylene (brake cleaner) will be superior? perhaps toluene? I think some experimentation will be necessary.


Lol. Believe it or not, I "am" a chemist. But though I try, it hasn't panned out, so instead I'm a self loathing unemployed hermit.

We need to get Piracetam's attention so he can come give us some pointers.


--------------------

"Now ether was substituted for chloroform, and the difference of their phenomena noted, and now some other exhilarant, in the form of an opiate or stimulant, was the instrument of my experiments, until I had run through the whole gamut of queer agents within my reach..."          I can do everything!!

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OfflineNoOneKnowsHowToAct
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Re: Potency Project [Re: Necco]
    #11816446 - 01/12/10 04:52 PM (15 years, 7 days ago)

I was also thinking of doing one of the simpler extractions like this one:
http://www.lycaeum.org/nepenthes/Extraction/extract5.html

I don't have chloroform though, so I was going to do a butane wash, an acetone wash, and if anyone thinks it'll help a naphtha wash before doing the methanol extraction.

This one also looked like it could work well:
http://deoxy.org/wiki/Mushrooms/Alkaloid_Extraction


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OfflineRoseM
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Re: Potency Project [Re: NoOneKnowsHowToAct]
    #11818046 - 01/12/10 08:27 PM (15 years, 7 days ago)

Thanks everybody for doing some leg work. If we can look at several teks and see which one is the best balance between ease and accuracy, we'll be on our way.

Perhaps we can find the easiest tek AND the most accurate, to use for the beginner and advanced studies.


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Re: Potency Project [Re: NoOneKnowsHowToAct]
    #11818758 - 01/12/10 10:10 PM (15 years, 7 days ago)

Quote:

NoOneKnowsHowToAct said:
This one also looked like it could work well:
http://deoxy.org/wiki/Mushrooms/Alkaloid_Extraction




I like the look of this one, and here is why (assuming it really works):

Even if the method is non quantitative we can standardize the process such that we can (hope to) assume standard loss. For instance, even if we are only extracting 55% of the alkaloids, if we can consistently lose 45% then the process will still work.

I've spent the last 5 minutes pondering and my brainstorm is this...
  • Add a standard number of grams, say 25g, of mushroom matter to a standard amount of ethanol (of some standard purity).
  • Mark container to take note of initial volume.
  • Heat for specified time in a water bath of specified temperature.
  • At the end of heating, add hot ethanol to bring to initial volume.
  • Using a large pre-weighed syringe with a filter attached, suck the ethanol extract through the filter into the syringe.
  • Place into a freezer of temperature x, for x time.
  • Remove syringe and attach a new (pre-weighed) filter, push the cold ethanol out through the filter and away from the crystals.
  • Allow filter and syringe to dry
  • Weigh syringe and filter (& crystals), subtract weight of syringe and filter to determine yield.

Who knows, it might work okay. One problem is that this method might only work for psilocybin. I haven't had the time yet to review the other posted links. Maybe I'll do that once this 2g batch of 60 minute acidified mushies I'm about to drink kicks in.

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OfflineLogicaL ChaosM
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Re: Potency Project [Re: Necco]
    #11819161 - 01/12/10 11:12 PM (15 years, 7 days ago)

Its funny you mention this, because I just bought some ethanol at a local liquor store for a mycelium extraction I'm going to do pretty soon...

I like that procedure mubba, but I'm confused on what the syringe is for. Is it for separating the aqueous ethanol from the "cooled" Psiocybin crystals? Is evaporation of the solvent/solution not even needed in your technique?
-----------------------------------------------------------------------------------

I see some Pro's and Cons using ethanol as a solvent for extracting the alkaloids:

Pros

- High-proof Ethanol is relatively common across the US, and likely across the world.

- This extraction method is the simplest simple. It only uses one chemical: the high-proof ethanol. Simple is good for this community-wide experiment.

- If those extracted crystal are given to trippers (after they have been weighed), for the "Potency determined by Subjective Trip Reports" part of the experiment, there is no danger of accidentally poisoning the tripper, unlike a methanol extraction.

Cons

- High-proof ethanol (190 proof or above) is not available everywhere. In fact, its illegal in some states in the US. That could cause some growers unable to do this extraction part of the experiment, unless they want to make some (nah, too much work).

- Alcohol is regulated by age limits. This means any growers under 21 will not be able to do this extraction method. That's a lot of users here. Unless, their older brother/sister/friend would like to lend a hand in the experiment...

- High-proof ethanol is extremely flammable! I should not that methanol is also flammable and its used for mushroom extractions, so this could be unavoidable. This could be dangerous to new growers who don't know proper safety measures for working with flammable solvents. Could result in injuries and unnecessary news coverage. That would be crazy...

- It requires a kitchen with a stove top. Likely all extractions will require some kind of cooking. Also, since the PF-Tek/grain both require a stovetop, I don't think this will be a problem for anyone who already grows. 

- Like mubba said, the yield is only about "55% of the alkaloids", which means it won't really represent how potent PE is to the Control, it will only show how potent PE is relative to another strain.
-----------------------------------------------------------------------------

Its still pretty good, considering the Cons. Maybe we could 2 different extraction techniques? Like anyone younger than 21 use one extraction method (like methanol), while growers 21 and up use this ethanol one. Then we average the results but only for the solvent they used and keep the data separate from each other.

I think that could work, that way more growers can participate in the extraction part of the project, which I think holds the most useful, unbiased and meaningful data of the methods proposed here.

Sounds good to me...
~ LogicaL Chaos ~

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OfflineRoseM
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Re: Potency Project [Re: LogicaL Chaos]
    #11819718 - 01/13/10 12:46 AM (15 years, 6 days ago)

Sounds good enough for a beginner's study!

Now for the advanced...


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InvisibleNecco
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Re: Potency Project [Re: LogicaL Chaos]
    #11819963 - 01/13/10 02:16 AM (15 years, 6 days ago)

LogicaL Chaos said:
"I like that procedure mubba, but I'm confused on what the syringe is for. Is it for separating the aqueous ethanol from the "cooled" Psiocybin crystals? Is evaporation of the solvent/solution not even needed in your technique?"


I suggested using a syringe because it is an easy way to get a relatively precise quantity of the extract. For this method to work we need to filter the hot ethanol really well, and the syringe will provide a way to do that quickly. The crystals will separate out of the ethanol as it cools while still inside of the syringe; when the crystals have separated out, another filter on the syringe will keep the crystals inside the system, while we push the spent ethanol out. No evaporation is necessary aside from letting the wet crystals dry, which is one of the reasons I'm fond of this route.

Worth mentioning: we do not need to filter the entire batch, just the amount that fits into the standard syringe size we choose. This is also a great facilitation.

"- High-proof ethanol (190 proof or above) is not available everywhere.

This is true, for instance, it is not available OTC in my state. While not ideal, denatured ethanol could serve as a substitute for those who cannot find other ways. This is :thumbdown: because you couldn't nom the crystals afterwards.

Of course, distilling liquor is a pretty neat challenge too! I remember having good old times back in my teens, soldering copper pipes together to create my first reflux column. <sigh> Now I can open my cabinet and pull out a jug of USP absolute; things simply aren't the same.

"Alcohol is regulated by age limits."

I'm pretty sure mushrooms are illegal to possess for people of any age. :wink: Okay, I just had to say it.

"High-proof ethanol is extremely flammable!"

This method circumvents others that use solvents such as diethyl ether, chloroform, hexane, etc., most of which are far more hazardous. It is actually quite easy to put out an ethanol fire compared to a naptha fire.

"Like mubba said, the yield is only about "55% of the alkaloids", which means it won't really represent how potent PE is to the Control, it will only show how potent PE is relative to another strain."

Yeah, the true psilocybin content of the mushroom will remain a mystery. The only thing we will discover is the content relative to one another. This could possibly be remedied by using some type of "known." How we would do that is currently beyond me. Then again, I'm a little :crazy2: right now. BTW, I pulled the 55% out of my ass (as an example) just in case anybody might have thought that represented an expected value.

It would be a problem if our standard procedure was concentrated to the extent that we always had a saturated solution; then we would always get the same value. Cross your fingers that hot and cold ethanol have widely different psilocybin affinity. Argh, brain hurts. Perhaps I'll come back to this tomorrow.

(edit: to include last paragraph)

Edited by Necco (01/13/10 02:25 AM)

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Offlinelibertaire
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Re: Potency Project [Re: Necco]
    #11820324 - 01/13/10 06:56 AM (15 years, 6 days ago)

Quote:

"Like mubba said, the yield is only about "55% of the alkaloids", which means it won't really represent how potent PE is to the Control, it will only show how potent PE is relative to another strain."

Yeah, the true psilocybin content of the mushroom will remain a mystery. The only thing we will discover is the content relative to one another. This could possibly be remedied by using some type of "known." How we would do that is currently beyond me. Then again, I'm a little :crazy2: right now. BTW, I pulled the 55% out of my ass (as an example) just in case anybody might have thought that represented an expected value.

It would be a problem if our standard procedure was concentrated to the extent that we always had a saturated solution; then we would always get the same value. Cross your fingers that hot and cold ethanol have widely different psilocybin affinity. Argh, brain hurts. Perhaps I'll come back to this tomorrow.




I'm just curious why ethanol would only pull that certain percentage of the alkaloids from the mushrooms?  Is it simply because that's about how much the alcohol is capable of holding?  If so, wouldn't this be able to be remedied by doing multiple extractions into fresh alcohol until eventually the material stops yielding crystals, which once that occurs, it would indicate that you've pulled all of the alkaloids, thus giving you a full value of alkaloids for that sample?

In any case, it seems like we're pretty set here with procedure.  Now it's time to implement it...who'll be the first to try this out?  I have a flush of "normal" cubes about to be ready (columbian rust spore), I'll give this a shot once they're ready.  We should decide now on a set quantity that we should be testing so that when multiple people attempt it, it will be easy to compare notes.  What do you think we should set the quantity at?  3.5 grams? 5 grams? 10? What would be enough to get a decent reading on the alkaloid levels?

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Re: Potency Project [Re: libertaire]
    #11820373 - 01/13/10 07:21 AM (15 years, 6 days ago)

Quote:

"Like mubba said, the yield is only about "55% of the alkaloids", which means it won't really represent how potent PE is to the Control,
it will only show how potent PE is relative to another strain."





Which is the question being asked. :yesnod:

(But I know from experience that ethanol is very efficient. Close to 100% extraction of magic.)


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OfflineNoOneKnowsHowToAct
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Re: Potency Project [Re: Doc_T]
    #11820389 - 01/13/10 07:28 AM (15 years, 6 days ago)

If I had to do an ethanol extraction I would have to buy 151 proof and then have to use a desiccant to get it higher. I have a couple of ounces dry and I'm willing to use some, just let me know. I'm still trying the vinegar methods since I've already started with that.


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Re: Potency Project [Re: NoOneKnowsHowToAct]
    #11820436 - 01/13/10 07:54 AM (15 years, 6 days ago)

Any thoughts on the number we should set?  We should really decide on this before people begin their experiments.  I don't have that much available to use, so those that have ounces to waste, you should limit your amounts.  Just because you have that much to use doesn't mean that you should use it, I think a small amount like 5 or 10 grams would be enough to get an accurate assessment.

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Re: Potency Project [Re: libertaire]
    #11820526 - 01/13/10 08:25 AM (15 years, 6 days ago)

The amount of sample used is completely irrelevant to anything. Just scale your results to match your sample size.
Obviously, you get 'smoother' results by using a larger sample, to a point. But do what you can.


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Re: Potency Project [Re: Doc_T]
    #11820554 - 01/13/10 08:34 AM (15 years, 6 days ago)

Just found this, someone who's doing the methanol extraction might be interested in:

http://www.shroomery.org/forums/showflat.php/Number/10355362#10355362

Particularly troubling in this thread is a quote from rogerrabbit that says the following:

"PF was wrong.  The 'crystals' are useless salts. "

I believe that is in reference to an ethanol extraction, which if that's the case, that's pretty lame because that was the method I was planning on trying.  Does anyone think RR is right about this?  I haven't heard of any results from a bio assay of these crystals, so I have no proof either way. I hope he's wrong.

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Re: Potency Project [Re: libertaire]
    #11820566 - 01/13/10 08:37 AM (15 years, 6 days ago)

I got a lot of crystals the first time I extracted with ethanol, much more than the weight of the magic involved with that sample.
So yeah, ethanol doesn't extract only the magic.

But again, that's irrelevant. You'll get the same amount of non-magic extracting two different batches.
(If you use the same method- I didn't.)
But if one has more magic, you'll get that too.


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Re: Potency Project [Re: Doc_T]
    #11820574 - 01/13/10 08:39 AM (15 years, 6 days ago)

That's definitely a problem though, what are these other non-magic things that are being extracted?  How can we go about purifying the final result?

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Re: Potency Project [Re: libertaire]
    #11820579 - 01/13/10 08:40 AM (15 years, 6 days ago)

It's not a problem.
The question isn't "what is the exact chemical makeup of this sample?"
The question is "are these mushrooms more potent than those mushrooms?"

It's really not as hard as people are trying to make it.


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Re: Potency Project [Re: Doc_T]
    #11820598 - 01/13/10 08:46 AM (15 years, 6 days ago)

But at the same time, I would like to be able to consume my results, and if there are other things in the final extraction, I would like to know what they are.  Furthermore, it would be nice to be able to say "We found that on average PE has x% of alkaloids, while B+ had y%.".  We're trying to be as scientific as possible.

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Re: Potency Project [Re: libertaire]
    #11820635 - 01/13/10 08:54 AM (15 years, 6 days ago)

Quote:

libertaire said: But at the same time, I would like to be able to consume my results,




What could be in there that wasn't in the original mushrooms? :confused:
And this is what I mean- people are overthinking this.
It's just not this complicated of a question.

Think "Pepsi Challenge", if you are old enough to know what that is.

Quote:

libertaire said:
Furthermore, it would be nice to be able to say "We found that on average PE has x% of alkaloids, while B+ had y%.".  We're trying to be as scientific as possible.




That may be one way to sound 'scientifical'. But it's not more scientific than other methods.
Consider this "Of 375 cultivators polled, more than 75%  said that in their experience, PE seemed more potent on average."

How is that less scientific?


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Re: Potency Project [Re: Doc_T]
    #11820668 - 01/13/10 09:03 AM (15 years, 6 days ago)

Ok, I'm seeing multiple accounts that the crystals extracted in ethanol may or may not be alkaloids.  Someone who tested a match head sized sample said they were weakly active.  I think to be on the safe side, we should stick to methanol, but that's just my opinion.  Does anyone know if you can buy methanol in a local store, or would I have to get it online.  Also, are there any dangers I should be aware of?  I know it's extremely toxic, but is it on a watched chemical list or anything?

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