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OfflineManu_Ish
Black Morel


Registered: 08/21/22
Posts: 46
Last seen: 6 months, 4 days
Ascorbic acid, ethanol, defatting, buchner vacuum filtration
    #28233685 - 03/17/23 12:36 PM (10 months, 6 days ago)

I am getting great results just using warm water and ascorbic acid for my extraction method.

I am wondering if it is really necessary to add ethanol and water to a secondary extraction to defat the first extraction?

I can see the fats, and I assume sugars, in the extraction. They seem to already be precipitated out, possibly by the ascorbic acid and low pH? (3.5 pH).


I'm thinking I could just add the extract to a buchner funnel and flask with a vacuum pump to filter out the remaining particulates?

Or are the fats and sugars dissolved in solution and what I am seeing is some chitin flesh leaking from my muslin cloth bag used for extraction? The substance tends to floc/clump together, and when filtering by gravity, there is a white soapy residue left behind in my filter. I assume it's fat and sugar?

I want to use the buchner funnel and vacuum pump just because the gravity method is slow and not very efficient.


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Edited by Manu_Ish (03/17/23 12:38 PM)


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OfflineShu
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Registered: 11/20/11
Posts: 885
Loc: PA, USA
Last seen: 11 days, 5 minutes
Re: Ascorbic acid, ethanol, defatting, buchner vacuum filtration [Re: Manu_Ish]
    #28234066 - 03/17/23 05:45 PM (10 months, 6 days ago)

Re. Defatting / Buchner - what is your goal?

The soapy residue is likely mucilage and other polysaccharides.


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OfflineManu_Ish
Black Morel


Registered: 08/21/22
Posts: 46
Last seen: 6 months, 4 days
Re: Ascorbic acid, ethanol, defatting, buchner vacuum filtration [Re: Shu]
    #28236143 - 03/19/23 08:57 AM (10 months, 4 days ago)

Quote:

Shu said:
Re. Defatting / Buchner - what is your goal?

The soapy residue is likely mucilage and other polysaccharides.





Thanks for your response.

Really I am just going for more clarity and proper color in my extraction. It is pretty transparent, but still slightly opaque. I don't need to crystallize or anything.

And I figure, if I have less substances (colloidal particles) floating around in the extract, then that will be one less substance I have to worry about oxidizing. I try to extract as much psilocin as I can and then it oxidizes rather quickly once I evaporate most of the water, so I am going to start nitrogen flushing my container holding the final medicine/product.

The ascorbic acid won't prevent it from oxidizing while in the presence of air. I have to nitrogen flush. The potency is high the day I make the medicine, but within a week it is oxidized and the potency drops off. I see the medicine turn from a golden yellow to a brown amber color over the course of a week or so. My goal is to maintain the golden yellow color for at least 12 months. I am certain nitrogen flushing will do the trick.


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🌞 Light only shines while facing the dark 🌚


Edited by Manu_Ish (03/19/23 09:47 AM)


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InvisibleIcyurmt
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Registered: 04/02/20
Posts: 1,625
Loc: 5a
Re: Ascorbic acid, ethanol, defatting, buchner vacuum filtration [Re: Manu_Ish]
    #28236768 - 03/19/23 03:02 PM (10 months, 4 days ago)

Quote:

Manu_Ish said:
The ascorbic acid won't prevent it from oxidizing while in the presence of air. I have to nitrogen flush. The potency is high the day I make the medicine, but within a week it is oxidized and the potency drops off. I see the medicine turn from a golden yellow to a brown amber color over the course of a week or so. My goal is to maintain the golden yellow color for at least 12 months. I am certain nitrogen flushing will do the trick.




Are you protecting the solution from ambient light?

"From the data presented it is clear that light is detrimental to the stability of aqueous solutions of psilocin and psilocybin. It is also clear that the onset of this light induced decomposition of the standards is rapid upon exposure. We would therefore propose that when carrying out analysis of these compounds that the solutions should be protected from light at all times, including when awaiting analysis in an auto-sampler. This can be simply achieved as in our procedure here by covering the auto-sampler, alternatively individual vials could be foil wrapped."

That same study tried using nitrogen to reduce degradation but it wasn't successful without the additional protection from light.

"Attempts to reduce degradation of the psilocin and psilocybin involved (i) introducing nitrogen into the vial, (ii) placing each standard in ice prior to injection and (iii) refrigeration of the standards until required for analysis. This was unsuccessful in preventing degradation with multiple peaks still being observed after replicate analyses of a sample prepared using the above procedures."

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


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Hunt for the habitat not the mushroom.


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OfflineManu_Ish
Black Morel


Registered: 08/21/22
Posts: 46
Last seen: 6 months, 4 days
Re: Ascorbic acid, ethanol, defatting, buchner vacuum filtration [Re: Icyurmt]
    #28238859 - 03/20/23 09:33 PM (10 months, 3 days ago)

Quote:

Icyurmt said:
Quote:

Manu_Ish said:
The ascorbic acid won't prevent it from oxidizing while in the presence of air. I have to nitrogen flush. The potency is high the day I make the medicine, but within a week it is oxidized and the potency drops off. I see the medicine turn from a golden yellow to a brown amber color over the course of a week or so. My goal is to maintain the golden yellow color for at least 12 months. I am certain nitrogen flushing will do the trick.




Are you protecting the solution from ambient light?

"From the data presented it is clear that light is detrimental to the stability of aqueous solutions of psilocin and psilocybin. It is also clear that the onset of this light induced decomposition of the standards is rapid upon exposure. We would therefore propose that when carrying out analysis of these compounds that the solutions should be protected from light at all times, including when awaiting analysis in an auto-sampler. This can be simply achieved as in our procedure here by covering the auto-sampler, alternatively individual vials could be foil wrapped."

That same study tried using nitrogen to reduce degradation but it wasn't successful without the additional protection from light.

"Attempts to reduce degradation of the psilocin and psilocybin involved (i) introducing nitrogen into the vial, (ii) placing each standard in ice prior to injection and (iii) refrigeration of the standards until required for analysis. This was unsuccessful in preventing degradation with multiple peaks still being observed after replicate analyses of a sample prepared using the above procedures."

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




OK, perfect because this confirms what I had thought. No, I wasn't being consistent with light exposure or oxygen exposure. I was betting on the ascorbic acid working, and also just seeing what would happen.  I did read about the rapid oxidation in aqueous solutions, so this helps. And I read that ascorbic acid won't do much in the presence of oxygen.

I will definitely be keeping the extract away from both light and oxygen.

I will download the study as well.


Thanks!


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🌞 Light only shines while facing the dark 🌚


Edited by Manu_Ish (03/20/23 09:35 PM)


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OfflineLucisM
Nutritional Yeast

Registered: 03/28/15
Posts: 15,622
Last seen: 1 month, 27 days
Re: Ascorbic acid, ethanol, defatting, buchner vacuum filtration [Re: Manu_Ish]
    #28239579 - 03/21/23 12:45 PM (10 months, 2 days ago)

you might find better answers here


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