beerwiz
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Ergotamine extraction
Have some ergot extract with 50% alkaloids and tried to do an alkaloid extraction.
Added 100ml water to 20g of the powder and basified to pH 11.5.
I then added 100ml Naphta and got what seems to be an emulsion after stirring with a spoon by hand for 2mins. The upper naphta layer is mixed with
liquid brown drops/bubbles.
Should I still separate the naphta layer and then wash with a 2M HCl solution followed by basification to then filter out the alkaloids or should I
take another approach?
I'm at a loss on how to proceed with the alkaloid extraction any assistance is welcome.
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forgottenpassword
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I very much doubt that ergotamine is soluble in naphtha. Why did you not research the extraction method before you attempted it? You should look on
google patents -- it is an extremely well researched and patented area of chemistry.
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Bert
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Thread Moved
20-9-2014 at 08:35 |
beerwiz
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After about 20 minutes, what seemed like an emulsion fully separated and I was able to do a clean separation. Proceeded forth with and HCl wash and
separated the HCl. I then basified the HCl to pH 9 and saw crystals forming but I used too much aqueous HCl and what I got is suspension of crystals.
I will wait a day or so for them to settle and then decant. Any tips are appreciated.
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forgottenpassword
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The only tip I could give you is that ergotamine is insoluble in petroleum ether/naphtha.
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beerwiz
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Even when it is aqueous with an alkaline pH?
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forgottenpassword
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Yes.
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Actinium
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in the literature it talks about using U.V. while looking at a chromatography column to seperate the different mixtures seeing how Ergotamine glows
under such device.
Crudest way to seperate is using ethyl acetate eluted thru an active alumina column following the path with a U.V. lamp and allow to drip into 10x
Petroleum ether.
Here is a Patent method based of the LEK Tovarna Farmacevtskih of 1972.
Another method is the use of Bentonite which can be found at the Hydro store as "Hydrotone".
Also you have not given any information relevant to the source?
Ergot is a very broad term. Is it dried mycelia, Sclerotia, is it wild or domesticated?
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beerwiz
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Quote: Originally posted by Actinium  | in the literature it talks about using U.V. while looking at a chromatography column to seperate the different mixtures seeing how Ergotamine glows
under such device.
Crudest way to seperate is using ethyl acetate eluted thru an active alumina column following the path with a U.V. lamp and allow to drip into 10x
Petroleum ether.
Here is a Patent method based of the LEK Tovarna Farmacevtskih of 1972.
Another method is the use of Bentonite which can be found at the Hydro store as "Hydrotone".
Also you have not given any information relevant to the source?
Ergot is a very broad term. Is it dried mycelia, Sclerotia, is it wild or domesticated? |
It is dried and powdered sclerotia which is then extracted and concentrated to contain 40% alkaloids. I'm trying to extract the pure alkaloids.
"Process for isolation of ergot alkaloids from ergot US20070161795A1"
Following this patent I will now attempt:
Mix the powder with toluene 85% and 15% ethanol and filter and discard the filtrate.
Add 120 proof ethanol to the toluene and ethanol solution, separating and keeping the aqueous layer. Make the aqueous layer alkaline to pH 7.3 with
5% NaOH and extract with toluene again. Evaporate most of the toluene under vacuum at no more than 35 Celcius until you see crystallization. Filter
the crystals and dry them in a vacuum dryer at 60 C at 50 mbar of negative pressure. Or completely evaporate the toluene, but yes scraping off the
powder from a round bottom flask is a pain through the small neck opening.
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aga
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I dunno what an Alkaloid is, but i do know what "Cat Litter" is : mostly Bentonite.
Unsure if "Cat Litter" is what it's called outside the UK.
It's the dry granules you put in a tray for the cat to piss on.
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Actinium
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| Quote: Originally posted by aga |
I dunno what an Alkaloid is, but i do know what "Cat Litter" is : mostly Bentonite.
Unsure if "Cat Litter" is what it's called outside the UK.
It's the dry granules you put in a tray for the cat to piss on.
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Here in the good Ol' US of A we have cat litter as well and yes cats tend to piss on it time to time.
As far as Bentonite, it comes in a variety of forms and different salts.
The Hydroton is the commercially available for of expanded agrregate. I remember reading a process years ago that used such in aqueous solution of
mycelia to filter and recuperate.
@ O.P., you do realize that you need a good Kg of Sclerotia to get any amount of usable tartrate and by usable I mean meager and if you actually
manage to extract it.
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beerwiz
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| Quote: Originally posted by Actinium | | Quote: Originally posted by aga |
@ O.P., you do realize that you need a good Kg of Sclerotia to get any amount of usable tartrate and by usable I mean meager and if you actually
manage to extract it. |
I'm aware of the bentonite method but it is difficult to filter out. I prefer a simpler process.
Yes, the yield is a meager 2-2.5%. What do you think of my extraction method, got any tips before I experiment with another 20g of product?
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Nicodem
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| Quote: Originally posted by beerwiz | | What do you think of my extraction method, got any tips before I experiment with another 20g of product? |
My tip is to learn chemistry first and waste precious material latter.
Why would someone use "naphtha" for the extraction of something like ergot alkaloids? "Naphtha" is essentially as polar as ligroin, petroleum ether,
or any plain alkane.
…there is a human touch of the cultist “believer” in every theorist that he must struggle against as being
unworthy of the scientist. Some of the greatest men of science have publicly repudiated a theory which earlier they hotly defended. In this lies their
scientific temper, not in the scientific defense of the theory. - Weston La Barre (Ghost Dance, 1972)
Read the The ScienceMadness Guidelines!
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Actinium
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I agree with Nicodem, especially when dealing with this compound. Ergolines are temperamental and when mishandled tend to isomerize into inactive
product. Pet Ether is great to separate product from solution. there is so much literature out there its ridiculous. the U.V. lamp is mentioned in
many papers. David E. Nichols used a centrifuge to separate while using the U.V. to watch the fraction move thru the tubes, saw it in a documentary a
while back.
Did you pick all this Ergot? just wondering, as I have my own private patch that I pick at every summer although I didn't go this year.
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beerwiz
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If it isomerizes it's no issue there's a simple procedure to convert to the active form. I have a friend who picks tons of it and processes it with
his milk machines. The centrifuge is good but unnecessary, you get a similar effect with a sep funnel. I wonder if the UV will damage the molecules, I
suppose a short 2-3 second burst won't do much damage.
[Edited on 21-9-2014 by beerwiz]
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