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an A/B improvement for MHRB extraction Options
 
picatris
#1 Posted : 10/31/2009 7:27:11 PM

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What I'm going to describe is basically a compilation of others' ideas, but there is a new step which may be actually a way out of the quagmire of low yields and impossible emulsions. Any comments are VERY welcome!

So far this has been performed on only 50 g. batches, but the method probably works for other quantities.

Step 0. Grind the MHRB as thin as you can. A Thermomix (TM-1) is great for that, but anything that grinds it to fine dust is OK

Step 1. Boil the MHRB with a solution of HCl with a pH of 2-3. The amount of water is unimportant (it will show up later why this is so). An electric hot plate can be used set at low temperatures so that it just simmers constantly. When the amount of fluid is low, remove it from the boiling pan and set it aside, adding more HCl solution. HCl is suggested as it is a volatile acid, which means it should not decrease the pH too much when the amount of water is diminishing. Repeat this process until the liquid removed becomes very lightly colored.

Step 2. strain the remaining bark to recover the remaining water. Note that it is possible to use your hands as the acidity of the water should be quite acceptable to hand skin, and hand pressure is the best, but wash hands later to remove any acidic remains.

Step 3. [This the actual improvement, which allows skipping any defatting phase and removes any possibility of emulsion.] Pick up the acidic tea and simmer it thoroughly. The idea is to seek to remove any trace of water! This will produce a reddish black goo that if cold will become vitreous. The temperature must be quite low, so that the Spice present will not be ruined. If an electric hot plate is at hand set it at the lowest setting allowing for a barely noticeable simmer. Depending on the amount of water, it is possible to accomplish this in 2-3 hours. The total weight of goo for 50 g MHRB is expected to be about 40 g.

Step 4. Put the goo in a 500ml Erlenmeyer flask and add 300 ml of tap water and heat it up, mixing continuously until it starts to boil. do not let the goo to stay on the bottom for too long for it may burn! The Erlenmeyer is not necessary, but it will simplify the process as it has a very convenient shape for vigorous stirring later on, allowing to continue the next steps in the same recipient. To finish this step, make sure the goo is totally dissolved in in the water.

Step 5. While hot, add a Lye (NaOH) solution until pH is about 13-14(litmus paper (pH 1 to 14) for pH measurement is more than enough) Don't be afraid to spend litmus paper, it's not that expensive.

Step 6. After there is no more NaOH reaction, but while the solution is still hot - even too hot is good! - add 40 ml of Naphtha. stir energetically for 1 minute, let it stay still for a while and do it again 2 or 3 more times. As a consequence of this method (because of step 3?) the naphtha will separate cleanly and fast - 2 minutes are enough for a full separation!. A 10 ml syringe can be used to collect the naphtha which will be mostly transparent, without any tinge of color! Repeat the naphtha addition 2 more times using 40 ml each time. Every time the naphtha will appear clear almost as water. All the naphtha extractions were performed with the liquid very hot. If necessary heating it up a little on a hot plate.

Step 7. As usual on these methods, put the Naphtha removed on flask, put it on a freezer and let it sit there for 36-48 hours. At the end the magnificent snow appears on your globe. Remove the naphtha and pick up the spice which will be snow white.

Yields are expected between 0.5-0.6 grams, that is between 1.0 and 1.2%, which I dare say are quite reasonable.

On hindsight it is not like this is a new Tek, although i believe that the novelty of deep boiling (step 3) is an important improvement in A/B extractions, allowing to skip a defatting phase, virtually making emulsions impossible, and producing high yields, probably also contributing to the whiteness of the produced spice. It can also be made with over the counter products (in some locations at least Smile ). Furthermore only 3 recipients are used (a Pyrex pan, a 500 ml Erlenmeyer and a common flask)

...and Happy Halloween all Nexus' inhabitants!


PS. This is for educational purposes only. In fact despite written as an "how-to" method, the above is just a wild guess, the author never has done nor intends others to do alkaloid extractions from any type of vegetables


"The elfclowns of hyperspace are already juggling in the center ring. Hurry! Hurry!" T.M


 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
acolon_5
#2 Posted : 11/2/2009 2:26:42 PM

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I worry that the improvement step (reducing the acidic tea into a semi-solid) is going to hurt yields. Tryptamines in acidic solutions degrade somewhat quickly, by removing water you are upping the pH tremendously (esp using HCL). I think that people will find reduced yeilds, and longer times before spice can be had.

The defat you speak of is rarely used I think....as a quick recrystalization takes care of any oils left over.

These are only my thoughts and observations, I have NOT tried your method yet so cannot truly comment on it.
The Spice extends life
The Spice expands consciousness
The Spice is vital for space travel
___________________________________________________________________________________________________
Never underestimate the power of STUFF!


I am certifiably insane, as such all posts written by me should be regarded as utter nonsense or attempts to get attention.

I don't know SWIM and personally don't trust him at all. If SWIM is posting, most likely I will not respond...as I said, I don't trust the guy. YOU I trust, but never SWIM.
 
picatris
#3 Posted : 11/2/2009 5:20:17 PM

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acolon_5 wrote:
I worry that the improvement step (reducing the acidic tea into a semi-solid) is going to hurt yields. Tryptamines in acidic solutions degrade somewhat quickly, by removing water you are upping the pH tremendously (esp using HCL). I think that people will find reduced yeilds, and longer times before spice can be had.

The defat you speak of is rarely used I think....as a quick recrystalization takes care of any oils left over.

These are only my thoughts and observations, I have NOT tried your method yet so cannot truly comment on it.


Your observations are pertinent. There is only one way to find out if this step is really useful. I have a methodical Slave Elf who is willing to make an unbiased experimentation with and without step 3, using 50 g of MHRB for each case. I'll post the results here both on yields and processing times

"The elfclowns of hyperspace are already juggling in the center ring. Hurry! Hurry!" T.M


 
acolon_5
#4 Posted : 11/2/2009 7:14:22 PM

The Great Namah


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Sounds good...only a side by side comparison can really tell us if the new steps are an improvement or not.

I eagerly await the results!
The Spice extends life
The Spice expands consciousness
The Spice is vital for space travel
___________________________________________________________________________________________________
Never underestimate the power of STUFF!


I am certifiably insane, as such all posts written by me should be regarded as utter nonsense or attempts to get attention.

I don't know SWIM and personally don't trust him at all. If SWIM is posting, most likely I will not respond...as I said, I don't trust the guy. YOU I trust, but never SWIM.
 
PerPLexED
#5 Posted : 11/2/2009 7:16:58 PM
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You make a step to remove water, to add water in the next step...whats the point of reducing to resin?
"We are the analogies we believe." - PerPLexED

PerPLexED is a confused fictional creature.
He doesn't know that he is fictional.
He doesn't know what fiction is.
He doesn't know anything, really.
But strives to know it all.
 
picatris
#6 Posted : 11/2/2009 9:36:42 PM

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PerPLexED wrote:
You make a step to remove water, to add water in the next step...whats the point of reducing to resin?


For some reason, which I cannot fathom, reducing the tea to resin makes emulsions very difficult and the naphtha pulls very clean. Probably the oily stuff gets together in a sort of longer polymer which has reduced solubility in naphtha, diminishing also the chances of emulsions. This is a conjecture, perhaps any chemist might provide clues to why this is...

"The elfclowns of hyperspace are already juggling in the center ring. Hurry! Hurry!" T.M


 
PerPLexED
#7 Posted : 11/3/2009 12:40:19 AM
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picatris wrote:
PerPLexED wrote:
You make a step to remove water, to add water in the next step...whats the point of reducing to resin?


For some reason, which I cannot fathom, reducing the tea to resin makes emulsions very difficult and the naphtha pulls very clean. Probably the oily stuff gets together in a sort of longer polymer which has reduced solubility in naphtha, diminishing also the chances of emulsions. This is a conjecture, perhaps any chemist might provide clues to why this is...


maybe the smaller oil molecules evaporate while the larger oil ones that stay behind are too large to be pulled/accidentally get into your product
"We are the analogies we believe." - PerPLexED

PerPLexED is a confused fictional creature.
He doesn't know that he is fictional.
He doesn't know what fiction is.
He doesn't know anything, really.
But strives to know it all.
 
 
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