Blizzloo said:

Quote:

(...)
Well now you got in my head and I think I could do a heated vacuum vs unheated vacuum trial of the liquid teas. Then combine the resulting teas to do the dehydrating temperature comparison. That would save some time and materials I suppose.

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I look forward to seeing the results

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It looks like heat plus vacuum was less efficient than vacuum alone.

Vacuum vs Heat Plus Vacuum extraction results.
Steps:
I boiled 4000 ml water for 15 minutes to de-oxygenate.
Then put 500 ml into a 2000 ml jar to cool and 500 ml into another for the heated test. Both with lids on so water vapor would displace air and create a vacuum as it cooled to limit o2 absorption into the water.
I split 100 grams of dried materials into two equal 50 gram bowls.
When the vacuum only jar had cooled to 77f(25c) and the heat plus vacuum jar had been reheated to 203f(95c) I added the 50 grams of dried active materials to each and pulled a vacuum on each setting a timer for 15 minutes.
I thought it was interesting to note that pulling the vacuum on the heated jar caused the solution to boil intensely at first and continuing at a simmer for the entire 15 minutes. That proved that the vacuum held as the jars sat at ambient temperature.
Both jars were shaken at 3 minute intervals.
At 15 minutes the vacuum only jar was still 25c while the heat + vacuum jar had cooled to 61.6c but continued to boil until the seal was broken.
The contents of both jars were filtered into separate containers using a french press.
Two samples of each were drawn from just below the surface of each using disposable pipettes and placed into sealed containers.
The samples were tested using Miraculix Qtests and standard procedures except that 0.4 ml of each were substituted for the normal 0.05 grams of dried material per conversations with the manufacturer of the tests for testing liquids.
While the indicated potency from the tests may be unreliable due to the liquid substitution, the relative potency between the samples should still give a reliable indication of which process produced better results.

The results were:
unheated vacuum only - 2.24 mg/g actives
heated plus vacuum - 1.77mg/g actives

Conclusion: I would not recommend heating plus vacuum for extractions. The additions of heat reduced the effectiveness of the extraction. This seems to confirm that heated extraction of aqueous solution is less effective than ambient vacuum extraction.

Part 2:
After completing the extraction steps above, the two teas were combined. Then the wet dregs of both batches were combined in one of the vacuum chambers with an additional 500 ml water and a vacuum pulled for a second decoction of 15 minutes. That decoction was filtered as before and combined with the first decoction tea to be used in the dehydrating temperature comparison to follow. Samples from that tea are drying now in a 60c dehydrator, a 60c oven, a dehydrator with the heating element disabled and in a still air dark chamber. They will be compared when the final sample is dry. These tests are for aqueous solutions of dried materials. Further testing will be required for drying of fruiting bodies at a later date.

Pix



Before preparing the qtests you can see that the vacuum only tea is more blue and the heat + vacuum tea is more brown.


Pre and post hot water bath.


Unheated vs heated results.

Dave Bennett said:

This paper looked into the stability of the alkaloids over time and found that they were stable in solution for two weeks (which was the length of the experiment, not when the the alkaloids completely degraded) if light was excluded and the solution was refrigerated.

Investigation into the temporal stability of aqueous standard solutions of psilocin and psilocybin using high performance liquid chromatography.

Bear in mind that it was written in 2005 when they didn't understand that psilocybin degrades into psilocin so the loss of potency, they found at seven days and traces at fourteen days has to an artefact of their handling process rather than the chemical properties of the alkaloids. 

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koma23 said:

I filtered the tea through a medium speed filter and at the end got about a 45% extraction. I'm guessing this is it in regards to a water based extraction. Any idea how we could reduce this?

...

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ReverendMyc said:

koma23 said:

I filtered the tea through a medium speed filter and at the end got about a 45% extraction. I'm guessing this is it in regards to a water based extraction. Any idea how we could reduce this?

...

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I love the removal while still in a leathery state. That looks so much nicer than the messy residue that my scraping results in.

As to the lab grade alcohol extraction, I found this paper on a method that a group of extraction enthusiasts have worked out. It requires some serious tech and chemical access, but is purported to be very effective. I am inserting the pdf and hoping that the Illuminati don't come for me.

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Ah yes, it really simplifies the process.

Regarding the alcohol precipation, I wouldn't call it "lab grade" It's just mixing the two together (the reduced water extract and alcohol), waiting an hour or two for the "solids" (precipate) to form and then filter.

I see you attached an alcohol extraction method (tnx), but what I'm referring to is not an alcohol extraction; it's an alcohol purification of the water extract. As far as my research goes in to alcohol extractions, you need to use a lot of alcohol (absent sonication), so it's not really economical, and I don't want to mess with methanol. Doing it this way is much cheaper. I'm going to try this today or one of these days.

As far as your testing goes I think the most important unanswered questions revolve on the subject of reduction; temperature, time, light ... Can you reduce on the stove at basically 100c or is keeping below 70c a must? How much does light exposure affect the final potency, etc.

A question about a prior measurement of yours. I was looking at the measurements of golden teachers. 400mg actives in tea and 47mg remaining in the dregs. That's 447mg in 25g of mush which equals to 1.79% actives in dried material. Am I getting something wrong? If not, that is a hell of a lot for GT. Have you thought about this yet?

Dave Bennett said:

Actionsaurusrex asked a question about the stability of the alkaloids in solution and I provided them with some scientific research pertaining to their question. Is mycological research banned in this thread?

And as to gummies not being a very good medium for psilocybin stability during storage anyone can Google "Do psilocybin gummies lose potency and why?"

Your latest experiment had some interesting results.

unheated vacuum only - 2.24 mg/g actives
heated plus vacuum - 1.77mg/g actives

Haven't you just proved that heat degrades potency?

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koma23 said:

...
A question about a prior measurement of yours. I was looking at the measurements of golden teachers. 400mg actives in tea and 47mg remaining in the dregs. That's 447mg in 25g of mush which equals to 1.79% actives in dried material. Am I getting something wrong? If not, that is a hell of a lot for GT. Have you thought about this yet?

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ReverendMyc said:

koma23 said:

...
A question about a prior measurement of yours. I was looking at the measurements of golden teachers. 400mg actives in tea and 47mg remaining in the dregs. That's 447mg in 25g of mush which equals to 1.79% actives in dried material. Am I getting something wrong? If not, that is a hell of a lot for GT. Have you thought about this yet?

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Sorry Koma23 - Can you link the post you are referring to? It is perfectly possible that I made an error posting or somewhere else. Hopefully I still have the data lying around if it is something older.

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ReverendMyc said:

Blizzloo said:

Quote:

(...)
Well now you got in my head and I think I could do a heated vacuum vs unheated vacuum trial of the liquid teas. Then combine the resulting teas to do the dehydrating temperature comparison. That would save some time and materials I suppose.

---

I look forward to seeing the results

---

It looks like heat plus vacuum was less efficient than vacuum alone.

Vacuum vs Heat Plus Vacuum extraction results.
Steps:
I boiled 4000 ml water for 15 minutes to de-oxygenate.
Then put 500 ml into a 2000 ml jar to cool and 500 ml into another for the heated test. Both with lids on so water vapor would displace air and create a vacuum as it cooled to limit o2 absorption into the water.
I split 100 grams of dried materials into two equal 50 gram bowls.
When the vacuum only jar had cooled to 77f(25c) and the heat plus vacuum jar had been reheated to 203f(95c) I added the 50 grams of dried active materials to each and pulled a vacuum on each setting a timer for 15 minutes.
I thought it was interesting to note that pulling the vacuum on the heated jar caused the solution to boil intensely at first and continuing at a simmer for the entire 15 minutes. That proved that the vacuum held as the jars sat at ambient temperature.
Both jars were shaken at 3 minute intervals.
At 15 minutes the vacuum only jar was still 25c while the heat + vacuum jar had cooled to 61.6c but continued to boil until the seal was broken.
The contents of both jars were filtered into separate containers using a french press.
Two samples of each were drawn from just below the surface of each using disposable pipettes and placed into sealed containers.
The samples were tested using Miraculix Qtests and standard procedures except that 0.4 ml of each were substituted for the normal 0.05 grams of dried material per conversations with the manufacturer of the tests for testing liquids.
While the indicated potency from the tests may be unreliable due to the liquid substitution, the relative potency between the samples should still give a reliable indication of which process produced better results.

The results were:
unheated vacuum only - 2.24 mg/g actives
heated plus vacuum - 1.77mg/g actives

Conclusion: I would not recommend heating plus vacuum for extractions. The additions of heat reduced the effectiveness of the extraction. This seems to confirm that heated extraction of aqueous solution is less effective than ambient vacuum extraction.

Part 2:
After completing the extraction steps above, the two teas were combined. Then the wet dregs of both batches were combined in one of the vacuum chambers with an additional 500 ml water and a vacuum pulled for a second decoction of 15 minutes. That decoction was filtered as before and combined with the first decoction tea to be used in the dehydrating temperature comparison to follow. Samples from that tea are drying now in a 60c dehydrator, a 60c oven, a dehydrator with the heating element disabled and in a still air dark chamber. They will be compared when the final sample is dry. These tests are for aqueous solutions of dried materials. Further testing will be required for drying of fruiting bodies at a later date.

Pix



Before preparing the qtests you can see that the vacuum only tea is more blue and the heat + vacuum tea is more brown.


Pre and post hot water bath.


Unheated vs heated results.

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ReverendMyc said:

Ahh. Yes. I had not actually caught that. So a couple of things here.

The samples came from the higher of these two tests which came out to 1.556% actives which is indeed very high for GT. Especially since it was an old powdered sample.
https://www.shroomery.org/forums/showflat.php/Number/28960154#28960154

I have mentioned that the absolute values of the tests are also suspect. I know I have mentioned the reasons here and there, but maybe not all of them in this thread or open forum discussions. Here are a few reasons.

The tiny amounts required for the bulk tests of 0.050 grams for standard samples and 0.025 grams for potent materials is at the very limit of my consumer scales. I use the one that the test manufacturer recommends and calibrate it often, but it is still limited.

The second reason is likely due to the "blanking" step for the colorimeter. The manufacturer now recommends heating the blanking sample used to zero out the colorimeter for the most accurate results. When I started all of these tests, that step was not included in the instructions so I was probably not starting from a proper zero. Now, when doing a comparison test, I still do not incubate the blanking sample to save on materials. But when I do actual potency tests for things like the myceliated grains over time trials or testing a new cultivar of semps or pans I do waste some of the extraction and reaction solution for the greatest possible absolute accuracy. But that is still only to within the tolerances of the scale and the colorimeter.

There could be other things as well like the +/- 5% accuracy of the colorimeter.

However, when I do these tests, I am using the same scale, blanking samples, and colorimeter for every test. So while the absolute values of the test results may be off, the relative potency between tests done at the same time should be reliable.

Best I can do for citizen science. Though I wouldn't be mad if Santa brought me an HPLC for x-mas. Unfortunately I must be on the wrong list.

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ReverendMyc said:

Well, I have gone through notes and calculations and the pictures from that time and everything looked right until I found a picture of a scale showing 50 grams of dry product and the two jars with dry mush powder in the bottom of each. It looks like I planned to use 25 grams in each but then actually decided to use 50 grams in each jar. I found a picture that appears to show one amount in two jars and then a second picture with double the amount.

If that is the mistake, then the total actives make a lot more sense. 0.447mg/g / 50g gives 0.894%. That is still at the top of range for GT but not unheard of per the 2021 psilocybin cup. The top GT that year was 0.84 total of psilocybin and psilocin. Miraculix Qtests also measure the combined total of psilocybin and psilocin. The large print on the boxes do not mention that, but Dr. Felix has confirmed it several times.

I cannot definitively say that this is what happened, but it does fit the evidence better than anything else I can come up with. In any case, that is a really good catch, so thanks.

I didn't think that I had any more of that sample left, but I just discovered that I do still have that exact sample in a drawer. So I am going to run a potency test on it again while I am doing the dried tea temperature comparisons when the last one finishes drying. I do have some better tools than I started with, so maybe I can get a more reasonable absolute potency.


Pictures from 2024-12-02, the day of that test.


P Cup info


Sample I just found that I still have.

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