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Little to no yield from MHRB. Is it something I did?

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Phenylthalatryx

Phenylthalatryx

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SWIM has been lurking in the forums, around the web, for about 2 months. SWIM had reasonable success with cactus extraction and thought it a good idea to try some MHRB.

First attempt went as follows:

About 100g finely powdered bark with about 500 ml of methanol refluxed in a soxhlet for about 2 days.

Methanol was evaporated off to leave a dark red sticky tar.

Tar was dissolved in 500 ml of acidic aqueous solution (Hcl and Distilled water adjusted to a PH of ~2).

Added a couple table spoons of activated carbon to solution and stirred under low heat. This was an attempt to remove some impurities because activated carbon doesn't absorb salts.

Filtered out carbon with buchner funnel and adjusted solution to a PH of ~8.5 with an aqueous solution of Sodium Hydroxide.

500 ml of VM&P naphtha was added and solution was shaken.

At this point everything just descended into utter chaos. A thick, foamy, pink emulsion from hell! It would not break up. Tried salt, tried water, tried heat, tried time. Nothing helped.

SWIM removed what naphtha he could and evaporated. Left what looked like soap scum on the bottom of the dish. When scrapped together it was oily yellow and about the size of a pin head.

SWIM cut his losses and chalked it up to a learning experience.


SWIM has since tried changing up his methods.

Tried going strait to base from the tar using much higher PH levels (about 12). That helped with the emulsion immensely.

Tried freezer precipitation in naphtha, but could not get crystals to form.

Tried using using activated carbon to absorb the alkaloids after going basic. This is an interesting technique. SWIM has never heard of anyone using it in any tek, but in theory it should work. Alkaloids, in salt form, are not absorbed in activated carbon but, in basic form, they are readily taken up. In theory you can add AC to the acidic solution to remove some of he impurities. Filter off the carbon and discard. Then, after you turn your solution basic, add activated carbon again to absorb all the alkaloids. Filter off all the carbon and retain. You should have all the alkaloids trapped in the AC. Add the carbon to a highly acidic solution. This should release the alkaloids from the AC by turning them back into a salt. You will have a very clean and clear solution.

Has anyone tried this technique or have any other advise for SWIM?
 
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are the salt forms of dmt soluble in methanol? because if you just ran the methanol through the soxhlet without freebasing..maybe its not picking up any dmt at all..and what you got is actually just oils?
 
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Salts are ionic compounds, and thus they are soluble in polar solvents like water, ethanol, isopropanol and methanol.

Because of the presence of tannic acid in wood, SWIM assumes that DMT in MHRB exists as a tannate.

A methanol extraction should pull out all salts, sugars, tannins, esters, and alcohols. Refluxing in the soxhlet is performed until the solvent comes out clear.

SWIM chose methanol because it is one of the best polar solvents and it has a very low boiling point (65.7 deg C). That makes it easy to evaporate. :)
 
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Phenylthalatryx said:
Salts are ionic compounds, and thus they are soluble in polar solvents like water, ethanol, isopropanol and methanol.
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Not all salts are soluble in alcohols. Tell SWIM to dissolve sodium chloride in methanol and see. SWIY needs to consider what solubility means, i.e. what happens to a substance when it dissolves in a solvent. In other words, to investigate what "dissolve" means.

Phenylthalatryx said:
Because of the presence of tannic acid in wood, SWIM assumes that DMT in MHRB exists as a tannate.
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Bad assumption. Chloride, sulphate, phosphate, acetate, oxalate, succinate, citrate, fumarate, malate, whateverate, are also present in the bark. Why exactly did SWIY decided that dmt forms a salt with tannic acid?

Phenylthalatryx said:
SWIM chose methanol because it is one of the best polar solvents and it has a very low boiling point (65.7 deg C). That makes it easy to evaporate. :)
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The word "best means nothing. Best for what? Water is more polar than methanol.

SWIM thinks SWIY complicates things too much. People have amazing success using just water, sodium hydroxide and naphtha. A pH of 8.5 may be **grunt** OK, but higher is better. At pH of 8.5 37.5% of the spice is going to be freebase and 62.5 will be salt.

Which of course would result in the first pull to be not good.
 
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A MHRB extraction can be a very simple thing. No lab equipment is needed (although may be helpful).

You may want to try something a bit simpler first, and then use your chem knowledge to "spice" your extraction up a bit to see if you can improve on the tried and true methods of extraction. Many of us have been doing this for a long time and have tried many methods. A simple A/B using a crockpot, a strainer, a few milk jugs, naphtha, vinegar, and sodium hydroxide have always provided me with the best results.
 
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Please forgive my presumptuousness.

DMT tannate, I suppose, is not the only possible salt form in MHRB.

I did not mean to disparage water as a solvent. It is certainly is one of the best.

However, sodium chloride is marginally soluble in in methanol (though not nearly as much as in water).

The soxhlet apparatus allows the same batch of solvent to be freshly cycled through the sample thereby negating the marginal solubility and allowing for a more complete extraction with much less solvent.

SWIM chose methanol mostly for its low boiling point. SWIM did not want to expose the spice to excessive temperature.

SWIM also chose the soxhlet because SWIM has had very bad experiences filtering out veggie matter.
 
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fourthripley said:
Our own Noman (where be he?) has successfully made cold methanol extractions from mhrb. I don't think that's where the problem lies.
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I did not even imply that methanol is not a good solvent for spice extraction. I just argued the statement that methanol is a good polar solvent that can dissolve salts.

Methanol is reported to be OK by some. SWIM has never used it for spice extractions though.
water on the other hand is more accessible and it is used all the time with success.
 
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