Harmala Extraction - Take Two

[Tryptallmine]

Hey All,

I started with my first harmala extraction the other day. I have a few queries.

The boils x4 + basing went well, color change and precipitation was noted.

Redissolved back into vinegar and saturated with 100g of salt to the litre of water to see more precipitation which I have filted to 9 grams of what I'm assuming is crude harmalas.

Very very fine needle crystals formed through the solution (that I have kept). They seem to be impossible to filter.

I'm wondering If I should redissolve it in water and base it again? Does this look right?

The paste/clumps have a vinegar odor.

 

[Tryptallmine]

I redissolved it in a small beaker with hot water - there was enough residual vinegar within the paste to get the pH acidic. I've just stirred in a couple of teaspoons of sodium carbonate and it is precipitating lighter colored harmalas.

A shame I threw the other half of the extraction out. The pH was 13+ and there were at least 50% more harmala's sitting at the bottom that I couldn't filter. Irrespective 5-7g of harmalas is plenty to experiment with considering a gram of DMT lasts me the better part of a year.


Q: Since we've already salt saturated to break up the other alkaloids is there a requirement to keep salting it? Or does it continually improve purity?

 

[concombres]

:shock: Never had harmalas come out like that.

It seems to work best if you decent after basing & then re-dissolve in acidic solution, filter, & repeat a handful of times until there is no more sediment when dissolved in vinegar.

Save salt/manske step for when everything is nice & pure. I have always yeilded nice golden needles following the Tao of rue to the letter.

 

[Tryptallmine]

:shock: Never had harmalas come out like that.

It seems to work best if you decent after basing & then re-dissolve in acidic solution, filter, & repeat a handful of times until there is no more sediment when dissolved in vinegar.

Save salt/manske step for when everything is nice & pure. I have always yeilded nice golden needles following the Tao of rue to the letter.

Thanks, I keep getting paste. The paste I have now is ever lighter in color which is odd.
It's based at the moment. I'll post up a pic in a second.

It resembles putty almost.

Maybe there was too much salt in it?

 

[Tryptallmine]

The harmalas? (if we can call them that) on the right are from the 2nd basing. That is filtered base precipitate.

 

[dreamer042]

The harmalas? (if we can call them that) on the right are from the 2nd basing. That is filtered base precipitate.

What is the white one on the left?

The putty looks appropriate for wet freebase, and the right picture at the bottom looks right for the putty/freebase after it's dry.

 

[Tryptallmine]

The harmalas? (if we can call them that) on the right are from the 2nd basing. That is filtered base precipitate.

What is the white one on the left?

The putty looks appropriate for wet freebase, and the right picture at the bottom looks right for the putty/freebase after it's dry.

The left is just some cleaned up DMT. I dropped and smashed a vial yesterday and had to recrystallize - was getting it ready to put into a vial.

So you think that wet freebase is ok?

I've just left it on that tray to dry for the next few days. There is so much of it still precipitating. I put a small bottle in the fridge that I thought was spent, and its half precipitated with freebase - probably another 2 grams. There is also another 1lt bottle that is probably still full of alkaloids.

I threw the other 2lt bottle that was based with probably 10 grams of harmalas in it - couldn't be bothered trying to work with it.

So that FB is smoalkable with some dmt right?

 

[dreamer042]

The harmalas? (if we can call them that) on the right are from the 2nd basing. That is filtered base precipitate.

What is the white one on the left?

The putty looks appropriate for wet freebase, and the right picture at the bottom looks right for the putty/freebase after it's dry.

The left is just some cleaned up DMT. I dropped and smashed a vial yesterday and had to recrystallize - was getting it ready to put into a vial.

So you think that wet freebase is ok?

I've just left it on that tray to dry for the next few days. There is so much of it still precipitating. I put a small bottle in the fridge that I thought was spent, and its half precipitated with freebase - probably another 2 grams. There is also another 1lt bottle that is probably still full of alkaloids.

I threw the other 2lt bottle that was based with probably 10 grams of harmalas in it - couldn't be bothered trying to work with it.

So that FB is smoalkable with some dmt right?

Ah I figured that's wut it was. Yeah those freebase harmalas look fine. Those plates of dmt and harmalas are looking 100% smoalkable to me. :thumb_up:

 

[Tryptallmine]

Excellent, I appreciate your input and help.

It's always a bit difficult with the first extraction, as you don't always know if what you're seeing is correct. Seems all the entheogens I'm interested in I can now extract myself from natural sources which is fantastic.

I loaded up 100mg of freebase harmalas last night and gave it a whirl. I think there was a tiny bit of residual DMT in the pipe which wasn't a bad thing. It felt nice and dreamy and certainly got the carpet moving - a great head space.

I gave it about 4 good hits and there was still freebase powder in the pipe when I was done which leads me to believe there are still some impurities or sodium carbonate - although I only used less than a two teaspoons on the last base and it all precipitate nicely.

I might keep refining it over the next few days simply out of interest. I think its time to dissolve a 2:1 ratio of DMT to Harmalas and infuse it into a nice blend of herbs and try some real changa.

Thank you again.

 

[downwardsfromzero]

I've been cleaning up some rue tea that's been sat around on my shelf for a while now.

What I've found is that patience really helps. Letting things settle and then decanting is a lot less hassle than trying to filter too early.

Getting the pH down to about 3.5 seems to aid in coagulating all that fine, powdery crud that passes through normal coffee filters. I've been using 10% acid vinegar and 25% food grade vinegar concentrate, which really helps to keep the volumes down.

And a couple of pinches of bentonite (per cup) will greatly aid in getting a clear filtrate if/when it comes to filtration. Beware, if you've got dissolved CO2, the bentonite can make your solution jump/rear up out of the beaker!

I cleaned up a good litre of cloudy solution pretty quickly using a combination of these methods once I got round to it. Some of it had stood waiting for about two years and the fine particulates still hadn't settled out. That was using ground, lightly toasted seeds though.

As stated elsewhere, cleaning out all the insoluble particulates is a key step in successful rue extraction.

Shame you had to toss those 10g, although 2L is quite a lot to play around with. That's part of the reason I had an extraction sat on the shelf for so long. Somehow the New Year helped me resolve the issue

Smaller is better, I wouldn't dream of extracting more than 25g P. harmala because the volumes get to be a hassle.

Of course, if you follow Ouro and wap's No filter, No reduce Syrian Rue Extraction then most of my comments could be seen as redundant... ?

 

[Tryptallmine]

Well it seems that I've figured out where I went wrong last time as I misinterpreted part of the tek. After salting back the Harmalas I'd kept the impurities from the filters and redissolved them back into my liquid which is why it was terribly overweight and full of plant gunk and junk. All the filtering I'd done was pointless as I'd just dumped all the crap back in...

I've been doing this extraction slowly over the past few days and filtered it to the point where the salted Harmalas in liquid form would pass through 3 stacked coffee filters - performed the manske (50g NaCl in 500ml) and was left with some nice needles in the morning. The tea was a beautiful dark red color once the Harmala HCl's were redissolved in water.

I used a solution of Sodium Carbonate in boiling water instead of adding powder to the tea. The color change was a beautiful golden color with very clean freebase precipitate as seen in the pictures.

I'll do another run on it to clean it further and then separate the Harmine and Harmaline. This extraction is 100% on the money! Very happy.

 

[Jees]

50 gr NaCl on 500 ml water --> 10 gr/100 ml

I always go for 15gr/100ml.
the 10 could work fine if the concentration of alks is high, but 15 gives you a fairer chance for better yield in a wider range of possible alks-concentrations.

 

[Tryptallmine]

50 gr NaCl on 500 ml water --> 10 gr/100 ml

I always go for 15gr/100ml.
the 10 could work fine if the concentration of alks is high, but 15 gives you a fairer chance for better yield in a wider range of possible alks-concentrations.

Thanks Jees, that probably explains why there wasn't as much as I thought there was going to be. Only around 2.5gr dried from 80-100g of starting material. Also at a pH of 8.75 everything precipitated out. Nothing further precipitated beyond a pH of 8.75.

 

[DansMaTete]

... Also at 8.75pH everything precipitated out. Nothing further precipitated beyond a pH of 8.75.

All my attempts (with 2 differents source material) gave me the same result. I guess some batch don't contain much harmaline due to time of harvest or storage or something happens during extraction process. If someone has some clue, i'd be happy to hear about it.

btw, nice golden color

 

[Tryptallmine]

... Also at 8.75pH everything precipitated out. Nothing further precipitated beyond a pH of 8.75.

All my attempts (with 2 differents source material) gave me the same result. I guess some batch don't contain much harmaline due to time of harvest or storage or something happens during extraction process. If someone has some clue, i'd be happy to hear about it.

btw, nice golden color

What is the chance of the inverse being true? A lot of Harmaline and not much Harmine?

I dosed 150mg in a capsule last night and 45 minutes later I was fighting tracers for hours and feeling pretty spaced out with visuals.