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A/B versus CIELO cacti extractions (fail)


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#1 YoshiTrainer

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Posted 17 July 2021 - 10:51 AM

So after talking to my old and new friend about cacti, extractions, Mycotopia and other things, they hatched a plan after I left to try their hands at an A/B side by side with the new CIELO procedure by Loveall and Shroombee. This was done with untested pachanoi PC too.

Greenskeeper's A/B

https://mycotopia.ne...s/#entry1481541

Loveall and Shroombee's work

https://wiki.dmt-nexus.me/CIELO#

Unfortunately due to operator error during the CIELO, the final results are not likely true.

It started with them harvesting 5 columns of cacti, maybe 2.5"x18"ea? Slice away most of the white inner flesh. They then cubed them, tossed them in the dehydrator and ground them in a blender. The result, 174g powdered cacti to be split between the two experiments.

They started w/the A/B putting white vinegar and 87g cacti powder in the crock pot for 6 hrs x3 and water 3hrsx1. After cooling a bit, added the pectic enzyme and let sit. They drained it through a dish towel, squeezing to collect the liquid then they ran it through a funnel stuffed with a couple cotton balls. The cleaned liquid was boiled down to a quart and Greenskeeper's recipe was followed for the rest of the way. Unfortunately, during salting, the first was too acidic, 2nd was much better, 3+ was right on. They pulled 1.29g sticky residue before washing and 1.22g after the wash. Might need 1 more wash?

The CIELO procedure, the # were adjusted for 87g powder instead of 100g. The milky water was made and the cacti powder was mixed in. Before microwaving, it has a texture of mousse. After microwaving it was dryish and sandy. Unfortunately, this is where the error occurred (I believe?). If you look at the picture of the glass bowl after the microwave, you'll see a residue stuck to the side (pic 1). I think they should have done a better job scraping the side of the bowl in between microwave bursts. By the end of the saponification, the residue was stuck, scraping could not remove it so they tried to wash it with EA, no luck. Later, they said hot water took it off. If they'd been thinking, they would have collected the water and rerun it in a mini extraction.

Moving forward w/the CIELO, they had to decant the EA off of the paste so they added a couple extra pulls in there. All the pulls were done w/freezer cold EA except the last which was done w/warm. To make sure the EA extract was clean, after running through a coffee filter, they ran the combined pulls through a glass turkey baster stuffed w/a couple cotton balls. Because of the extra pulls, they had more than a quart and used a 1/2 gallon mason jar to salt in. To be sure, they added 20g citric acid and swirled hard for about 3min. The jar was then placed in a quiet spot for about 20 hours. You could see a residue had formed but was stuck to the walls (pic 2). The salted EA was poured through a glass turkey baster w/cotton balls. The excess EA was blown out of the baster and the contents allowed to dry for a few minutes. Then warm water was poured into the mason jar and swirled for a minute then through the baster, collected and evaporated. Due to error, the end result, only 0.1g of salts. The salt tasted slightly salty, slightly bitter with a little sour in the finish.

Comparing the two procedures, CIELO is much safer, much faster and easier! Your whole extraction, up to evap, could be done in the time your are completing the acid phase of the A/B. I'm disappointed there cannot be a direct comparison of the yields do to operator error! Hopefully they'll do a proper comparison in the future. I think the next test will be using CIELO with freshly harvested columns.

The end products are beautiful! The citrate is a rose colored very fine crystal (pic 3). The HCl a lovely orangish, slightly tacky crystalline product (pic 4). Hopefully some experimentation......on lab rats :) ....... is in order!

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Edited by YoshiTrainer, 17 July 2021 - 10:59 AM.

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#2 bezevo

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Posted 17 July 2021 - 11:38 AM

that is really interesting ...i hope a cpl more people do another side by side extraction  like this so  as the scientist types say peer reviewed .confirmed

so we can go from theory  to undisputed proof for sure or fail  . almost there .

 

thanks bunch Yoshi for sharing these write ups .

 

bez


Edited by bezevo, 17 July 2021 - 12:04 PM.

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#3 Norman

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Posted 17 July 2021 - 03:08 PM

Yes thanks for doing this Yoshi.
I think I missed it - is there a point to the microwave beyond faster drying? If not, one could just spread their paste out on a sheet pan lined with parchment paper in a low oven for an hour or so.
Hopefully you saved your materials from the cielo procedure because there’s at least a dose in there somewhere to be had.
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#4 YoshiTrainer

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Posted 17 July 2021 - 03:41 PM

On the Nexus, in the long thread, where they worked on their experiment, I believe they provided a link to a previous discussion on the use of a microwave for saponification. I'll have to go back and follow the link, I have not read it yet. I think it is to break down the chlorophyll too? (Maillard?)

From the web:
"Saponification is a process that involves the conversion of fat, oil, or lipid, into soap and alcohol by the action of aqueous alkali (e.g. NaOH).[1])[2] Soaps are salts of fatty acids, which in turn are carboxylic acids with long carbon chains. A typical soap is sodium oleate."

The microwave looks like it did dry out the product and cook it at the same time causing a color change.

They did hang onto the used EA in hopes of something more coming about. I think the residue from the glass bowl that was washed down the drain was a major loss! The next time will be smoother.....hopefully! :)
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#5 Norman

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Posted 17 July 2021 - 04:29 PM

Did they mention anywhere why they want the material to saponify? That’s a bad thing with water based methods. Isuppose with EA it might not cause a problem, but why do they want it?

#6 YoshiTrainer

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Posted 17 July 2021 - 05:43 PM

Both of these are quotes from Loveall found on DMT Nexus.

https://www.dmt-nexu...g=posts&t=96262

"Differences with the microwaved paste:

1) When not microwaving, the solvent extract is a deep dark green in ethyl acetate. When the microwave is used, ethyl acetate picks up only a lighter yellow color.

2) Without the microwave step, a sticky precipitate formed in the jar walls during ethyl acetate salting. This was residue dried to a powder and picked up with a small amount of water. When acetone was added to this, a small ammount shiny xtals form (like in dg's dual solvent xtalization process). Presumably, this powder was is mostly other stuff that trapped some mescaline sulfate (wich otherwise is caught by the filter).

3) Without the microwave step, the filter paper has multiple rings in it (see image below). I think this is an indication of several different biological compounds in the ethyl acetate (including the deep green residue with Rf = 1 at the rim of the filter paper). This is a lot messier than the single ring seen on the microwaved process (the one seen in post #2 with Rf ~ 0.3). With the microwave step, the deep green in the extract is not present."



"It seems the microwave breaks down complex plant parts into simpler ones making the ehyl acetate extract cleaner.

One interesting thing about the microwave (which I think you don't have) is that we may be doing something called Microwave Assisted Saponification (MAS).I believe it breaks down esters (generally soluble in ethyl acetate which is itself an ester) into carboxylate ions and organic alcohols. An important example is,

Chlorophyll + 2OH- ⇒ Chlorophyllin-- + Phytol + Ethanol


So less matter is soluble in ethyl acetate. In the example above, assuming ethanol mostly evaporates, only phytol is available for ethyl acetate to pick up. It has an amber color (apparently) and when extraction at 0F it does not appear to be picked up (since extract is colorless)."


Here is the link they offered for Microwave Assisted Saponification.

https://www.dmt-nexu...450#post1062450

#7 YoshiTrainer

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Posted 17 July 2021 - 06:37 PM

From Wikipedia

"Ethyl acetate hydrolyses to give acetic acid and ethanol. Bases accelerate the hydrolysis, which is subject to the Fischer equilibrium mentioned above. In the laboratory, and usually for illustrative purposes only, ethyl esters are typically hydrolyzed in a two-step process starting with a stoichiometric amount of a strong base, such as sodium hydroxide. This reaction gives ethanol and sodium acetate, which is unreactive toward ethanol"

Maybe this is also why they are evaping the water?

#8 YoshiTrainer

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Posted 19 July 2021 - 01:53 AM

1.07g HCl salt after second wash using freezer cold acetone, a small glass and back of a metal spoon for mashing the salts. It was all drained through the glass turkey baster stuffed with a couple cotton balls and rinsed with more cold acetone. The baster was blown out and allowed to dry before warm water was poured through and collected on a glass plate for evap.

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#9 Norman

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Posted 19 July 2021 - 02:42 AM

Truly beautiful work there.
Seems to me that you have A/B down pat so I’m double mystified at your looking elsewhere.
To be honest though I do see the allure of the road not taken. It’s cool getting something to work the way nobody else has yet.
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#10 YoshiTrainer

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Posted 19 July 2021 - 09:19 AM

Thank you very much Norman! The A/B could use a little more practice for a cleaner end product (too acidic of a salting). Certainly, many of use here are drawn to experimentation, I think it is part of who we are. If the CIELO procedure gives worthwhile % of end product, it is so much easier, safer and faster than an A/B. You also only need basic kitchen equipment, a few Mason jars, plate for evap, microwave, coffee filter, lime, EA, citric acid and cacti.

I think the next test will be freshly cut PC instead of dried powder. We were debating whether to add NaCl to the freshly blended cacti before starting CIELO?

#11 Norman

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Posted 19 July 2021 - 10:32 AM

I’d get a decent yield out of the CIELO as written before I started changing it up.
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#12 YoshiTrainer

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Posted 21 July 2021 - 02:01 PM

This mini experiment was to test whether fresh cacti could be used w/Loveall and Shroombee's CIELO procedure. Starting at 9:15 am with collecting pups and other young leftovers from the experiments posted above. They (604g) were rinsed, chopped and run through a food processor, core and all. (pic 1) The cacti mush sat for an hour with NaCl added which is not part of CIELO and was probably unnecessary. Lime was added, it was stirred for 10 min and rested for another 8 min. (pic 2) Then the microwaving started in 39s intervals with stirring and scraping the bowl in between. After driving off a bunch of water and changing the color of the cacti mush, it was cooled for 30 min before the pulls started. (pic 3) First 3 pulls with freezer cold EA, last 3 with warm EA. The pulls were run through a coffee filter and then glass baster w/cotton balls.

By 2 pm, citric acid was being swirled with the combined pulls for salting. It took 4.75 hours, that was quick! In reality, at least an hour could have been shaved off the total time w/out the NaCl step and a little tighter procedure. After sitting for an hour the salted EA jar was checked and there was visible sediment. The jar was left for 20 more hours. The EA was then filtered through the glass baster w/fresh cotton balls. The empty jar and baster were allowed to dry. Warm water was used to rinse the salting jar then poured through the baster and collected on the evap plate. After evap, a clear dry residue was left behind. When scraped up, it was a very fine crystalline powder. (pic 4) The result, another .1g and more experience. The final pic is the results from the first (failed) attempt and the recent. (pic 5) Considering the starting material, I'd say this was a success. Next experiment will be A/B vs. CIELO again but with fresh green cacti skins.

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Edited by YoshiTrainer, 21 July 2021 - 02:14 PM.

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#13 bezevo

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Posted 22 July 2021 - 01:18 PM

This is  an amazingly simple process .. Yoshi  ......

Various other tek i have read are way more complex and labor intensive ..

i need to get my note book down and go threw this thread and get the steps down clear . in my note book  .

 

Thanks Yoshi

 

BEZ


Edited by bezevo, 22 July 2021 - 04:42 PM.

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#14 bezevo

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Posted 14 August 2021 - 03:17 PM

Has anyone else  done simalar comparisons



#15 Loveall

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Posted 17 August 2021 - 12:13 PM

Thanks for this work YoshiTrainer ❤

One open question we have with CIELO is, should be chemichally dry the EA before salting with citric? It could make the result a lot more robust for everyone. This is a standard lab technique to avoid any "noise" from water that comes along during the
solvent extraction.

We think CaCl2 deicer pellets or Arm and Hammer super washing soda (believed to be the Na2CO3 monohydrate) could do a good job at chemichally drying the EA in 30 minutes or so. Alternatively sarting with baking powder one could get dry NaCO3 using an oven (e.g. https://naturesnurtu...-washing-soda/)

I'll let you guys know when we get any new results. Cheers and thanks again
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#16 YoshiTrainer

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Posted 17 August 2021 - 01:14 PM

Thank you for the kind words and information Loveall!

Before neutralizing the used EA from both extractions, it was run through a glass turkey baster stuffed w/2 jumbo cotton balls. The baster was air dried then warm water was poured through, collected and evaporated. The residue left behind was a light brown goo (0.1g) that would not dry and had a very sour taste.




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