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THH extraction tek

Migrated topic.
Cheers' appreciated'
Shall know soon if absolute Methanol has the same effect as the first attempt in Methanol/Ethanol' or it was the methyl-violet that turned bright red'
The only other way around the sodium chloride would be to freebase the alks with ammonia solution'
Red or no red' it shall be tested for activity'

Bliss

Nobuoni +
 
LLB said:
you dont HAVE to pay taxes on it at all... heheheh...
not with the easy still... even a retard can make ethanol with this...
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HAHHA SWIMS FOAF got one of these...they are AWESOME...throw in the cheapest 50% alcohol vodka you can get..and boom a few hours later you have close to 95% ethanol...you make two mixed drinks from this stuff and you are toast!! and this comes from a serious alcoholic!! hehehe
 
Nobuoni said:
Cheers' appreciated'
Shall know soon if absolute Methanol has the same effect as the first attempt in Methanol/Ethanol' or it was the methyl-violet that turned bright red'
The only other way around the sodium chloride would be to freebase the alks with ammonia solution'
Red or no red' it shall be tested for activity'

Bliss

Nobuoni +
Click to expand...

Harmala red could even be more potent than harmaline. Who knows? I never heard of anyone testing it.
 
Ok, I gave the Ascorbic Acid thing a try.

A solution of ascorbic acid (300ml h2o/9g) was gently warmed until slightly bubbling then 1g of rue extract (slightly brown) was added. This was then gently heated for five hours with no colour change observed. An additional 9g of ascorbic acid was added gradually throughout heating.

Afterwards the solution was allowed to cool and then was rebased with sodium carbonate. Unlike before when the solution would turn a bright yellow this time it's a more dark/orangey colour.

Basically I have no idea what I have now. I was relying on seeing a colour change but after 5 hours it was getting late and I didn't want to leave it over night (plus it already had taken longer than expected). Once it has completely dried it will be weighed and tested sublingually.

Anyone else tried this yet?

Also does anyone know at what ph THH is expected to crash out of a solution?
 
soulfood said:
A solution of ascorbic acid (300ml h2o/9g) was gently warmed until slightly bubbling then 1g of rue extract (slightly brown) was added. This when then gently heated for five hours with no colour change observed.
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Nobuoni said:
The process slows down in acid solutions' but works faster in alkaline'
The stability of ascorbic acid decreases with increases in temperature and pH.
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soulfood, I would assume your solution was quite acidic with that amount of ascorbic acid in it? How much would an acidic environment slow this process down compared to an alkaline environment?
 
The inital ph was around 3-4 but as things went on I managed to balance the ph up to around neutral, oh yeah I missed this bit by adding a little sodium carbonate. I guess that was kind of important.


Once everything's dried up I'm going to make 2 solutions. 1 of standard rue extract and the other of the ascorbic acid treated extract. I'll make them slightly acidic and then add sodium carbonate dropwise and see if they precipitate at a different ph.

I'm wondering if the slight impurities in my extract in contact with the ascorbic acid may have something to do with the darker colour when I was expecting a clear one?
 
Nice one bro' the only way to tell if it had any effect on the Harmine is to test it'
No got that far as of yet' still cleaning the mole from the seeds'
Keep us posted as to any difference in effect from untreated alks'

Bliss

Nobuoni +
 
A dry extract salted out twice' brown yellow in colour was added to 50ml of Methanol'
The Methanol went instantly red/brown'
A most deffinite red colour'
Shall leave the Methanol to do it's job' then draw it off and evaporate'
Of whatever the result is' it shall be tested sublingualy'
The red/brown colour is the same colour as the boiled seed extract' except it has no yellow to it' as in the Harmala alkaloids present in the boiled seed extract'

So possibly another Harmala alkaloid reacts with the Methanol' making the bright red colour'

A test shall prove'

Bliss

Nobuoni +

Looks like you got to base crash the alks out !

Still no info on the pKa of THH'
Harmine 7.7
Harmaline 9.8

I am guessing here by the xlog of THH' it has a pKa somewhere at 8.5 ph' :)))
 
There are 22 alkaloids in Sirian Rue seeds'

Peganine (Vasicine)
Harmalol
2,3 - Trimethylene-4-quinazolone
1,2,3-(a-Hydroxy-trimethylene)-4-quinazolone
Oxodeoxypeganine
Oxopeganine
Tetrahydroharmine
Deoxyvasicone
2-Alkoxy-4-quinolone derivative
Deoxypeganine
Peganidine
Pegamine
Peganol
Ruine (8-Hydroxy-glucosylharmine
Deoxypeganidine
Dipegine
Isopeganidine
Vasicinone
Dyhydroruine (8 -Hydroxyglucosyl-harmaline
5- Hydroxytriptamine
6- Hydroxytriptamine
Harmol

Any one' or a combo of many could be the reason for the red in Methanol'
Only a test shall tell to it's activity'

Bliss

Nobuoni +
 
Nobuoni said:
Nice one bro' the only way to tell if it had any effect on the Harmine is to test it'
No got that far as of yet' still cleaning the mole from the seeds'
Keep us posted as to any difference in effect from untreated alks'

Bliss

Nobuoni +
Click to expand...

The thing is I never tried THH before and if it happened that only some of the extract was converted would I still notice the difference?
 
From all accounts a small amount should be slightly stimulating' unlike Harmine' of which is sleepy dreamy'
If the ascorbic acid had any effect' then it shall be noticable in your extract'

Bliss

Nobuoni +
 
Nobuoni said:
From all accounts a small amount should be slightly stimulating' unlike Harmine' of which is sleepy dreamy'
If the ascorbic acid had any effect' then it shall be noticable in your extract'

Bliss

Nobuoni +
Click to expand...

SWIM's always found harmine to be fairly stimulating but understands that it's actually harmaline that makes one sleepy/dreamy. THH is more centered, like something between a mild psychedelic and a nootropic. 69ron's posted his account of the difference between the three here: Harmala alkaloids for beginners? - Harmalas - Welcome to the DMT-Nexus. SWIM finds it to be quite accurate, though he has little experience with harmaline itself. The difference between THH and the other two is that THH lacks the mental cloudiness commonly experienced with them.
 
Ok' before I go and mes up another extraction from these seeds'

Would this be ok ?

Take the seeds whole and boil them 3 times in acidic water'
Strain'
Combine the solutions and reduce to about 300ml'
Let this solution stand for a couple of hours so all the sediment falls to the bottom'
Decant off' leaving any sludge in the bottom'
Add a few spots of ammonia solution to your solution to raise the ph'
The Harmine freebase crashes out of the solution and falls to the bottom'
Decant off gently'
Add hot water and mix real well' then filter'
Add a few spots of ammonia solution' to your solution' the freebase alks crash out'
Filter this solution and leave the filter to dry'
Scrape the alks off of the filter'

Attempts to clean the alkaloids with alcohol' came up dark redbrown' very fine dark powder'
As to it's activity' unknown at this time'

Bliss'

Nobuoni +
 
That's what I always wanted to do, omitting the salting out. For some reason it doesnt always work to well and I have to repeat it over and over to make sure everything comes out.

Can someone explain the point of the salting when repeated basing and filtering seem to clean up the alks pretty well? Does the salting favour the harmalas and neglect other alks in the seeds or something?
 
I would not omit the salt step... What trouble do you have with it? Just add excess salt (36g per 100l of liquid) and leave overnight in the fridge. Then decant/filter, and redissolve whatever precipitated/stayed on top of the filter in some more warm water and then freebase.

The salt step is the one that removes unwanted alkaloids such as vasicine and vasicinone. A friend of burnt from this forum tested and saw that the salt precipitated stuff indeed does not have those alkaloids, if Im not mistaken shulgin once tested the product from somebody who also did the same and was also free of those alkaloids

btw, nuoboni, you can just repeat the whole process over and over again a few times without the alcohol part, and each time will get a purer product. After the first run through, the filtering becomes much easier

Would be nice to know if the product from alcohol evaporation is bioactive, though... also if the same happens when redissolving freebase harmalas in alcohol or only their salts
 
endlessness said:
The salt step is the one that removes unwanted alkaloids such as vasicine and vasicinone. A friend of burnt from this forum tested and saw that the salt precipitated stuff indeed does not have those alkaloids, if Im not mistaken shulgin once tested the product from somebody who also did the same and was also free of those alkaloids
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Most of the time for me this is fine. But a couple of times after 48hrs refrigeration no precipitate whatsoever was seen. So I kept having to boil it down and re-saturate with salt then just a little came out each time after. I always make sure to salt the alks first time round but on the repeat cleanups I just filter and then rebase.



Anyway 50mgs ascorbic treated extract (ATE) sublingually gave no noticeable effect so 30 minutes later the same dose was repeated, then later 50mg original extract sublingual and another ATE 100mg oral followed by 70mg DMT fumerate (crazy dosing method I know).

What followed was a pharma trip that had had OEV's that were very clear, but with a very clear head (absolutely no cloudiness or looping) but a little short on duration although it seemed much longer. Usual dose 50mg DMT and 200mg harmala spaced apart 30 minutes.
 
I missed out that I would salt out after cooking down the seeds'
Then wash this mass of gunk in warm water' and filter it through cloth'
Then crash the alks out with ammonia solution'
Wash the next mass of gunk/crystals in hot water' dissolve it all' and filter'
Then crash the base alks out with ammonia solution'
One thing found' this is a vey time consuming plant to work with'
Also if you go too high with the amount of seeds you start with' you better consider a way of defating it all first'
Even if you no grind the seeds' you get one hell of a lot of gunk' of which eventualy gives you few grams of crystals'
Appreciate your input' litres' salting' crashing out in the fridge'
Serious filter papers and a vacumpump would no go a miss :)))

Just to add' the alkaloids washed fom the salting with Methanol' the dark red brown upon grinding has gone'
The resultant powder is dark mustard yellow brown and smells like coffee'

Testing it now'

Bliss

Nobuoni +
 
I tried using egg whites when I used 250g of seeds. Sure enough it cleaned things up but I'm wondering if I lost some of my yield as it only seemed to be a little more than when I did a 100g extract with just fridge decanting. But then again the 250g extract was cleaned a lot more. Either way I think next time I'm just going to be very patient and maybe take 2x as long with the fridge decanting. Maybe 4 days.
 
50mg under the tongue' dissolved there then swallowed'felt initial effects inside of 15 minutes'
Active'
Calm feeling' slight fuzzy head but awake' numbe tongue'impression of slight nausia'
The effect is most deffinitaly recognised'

So an active maoi of this extract would be 100-150mg ?

Dreamy' with energy' very nice ! !

Bliss

Nobuoni +

Um' you folks drink tea of Rue ??????

Phwaaaaaaa'~ :)))

No salt in this' an extremely bitter extract'

++++
+++
Decanted off after 1 day' then set the solution back in the fridge' there is another inch of alks and sludge' much cleaner yellow than the first crash after 1 day'
3 days now'
It seems this red/brown in Methanol' upon drying looks dark brown'
Upon grinding it becomes mustard yellow brown' the dark suff seems to coat the surface of the alks' no make any difference to activity though'
 
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