Trick to speed up Harmala extraction from Syrian Rue (using Gordo Tek)

[Rolinwama]

Hello,

So this post assumes the reader knows the famous harmala from syrian rue extraction tek which was presented by GordoTEK for example.

There is already one upgrade of the tek where you can just pressure cook the seeds in a sock using vinegar solution instead of grinding and boiling them - a lot less filtering needed.

During my extractions I have found another simple trick to speed this up:

At some point you are required to dissolve your freebased alkaloids in a hot vinegar solution and then add salt to it, enough for salt crystals to form but not too much so the crystals grow big. In all the guides it is said you have to go through this freebasing/salt crystallization few times (like 5 or so) to have the product purified.

The trick I have found out is that during the salting step, keep the solution in a hot (near boling/boling) water bath and add as much salt as possible (if there are leftover grains it won't be a problem) - just saturate the hell out of the solution with salt. Now the most important part: keep the solution in the hot water bath and wait.

What will happen after 30-40 minutes if you keep the solution hot: the salt form harmalas will remain dissolved in the solution (keeping in hot water bath will prevent harmala salt crystallization), yet the gunk will precipitate out! After separating the hot solution from the gunk and freebasing it (there is no need to wait for salt crystals to form then, it's quite pure already) you will get rather brightly colored harmala freebase. This was good enough for me - I did not require white product, very light beige is good enough. You could probably get it to white by one more cycle (instead of suggested 5).

It doesn't seem to ruin the yield (around 2% from rue), I also did bioassay and potency seems good - 50mg sublingual more than enough for a pharmachanga session. I think this is a good thing to consider when doing this time consuming extraction.

Oh by the way - do not approach this without proper buchner funnel filtering setup, I've learned the hard way... 80% of the extraction time was waiting for stuff to filter out, easily saved with proper vacuum filtering.

 

[Jees]

Hi Rolinwama,
great you are playing with possibilities :thumb_up:

...In all the guides it is said you have to go through this freebasing/salt crystallization few times (like 5 or so) to have the product purified.

A few manskes gives me a nicier yellow product indeed but some people are convinced that just 1 manske is really enough in terms of ridding the quinazolines effectively, so there is not 1 take on this. Since I do several A/B transitions (with filtering the acid stage) the alks are fairly clean and 1 manske suffice nowadays.

The trick I have found out is that during the salting step, keep the solution in a hot (near boling/boling) water bath and add as much salt as possible (if there are leftover grains it won't be a problem) - just saturate the hell out of the solution with salt. Now the most important part: keep the solution in the hot water bath and wait.

What will happen after 30-40 minutes if you keep the solution hot: the salt form harmalas will remain dissolved in the solution (keeping in hot water bath will prevent harmala salt crystallization), yet the gunk will precipitate out!

I also find gunk in the salted liquid (even when heading for 20gr salt/100gr liquid) , therefore I poor the very hot salt liquid trough a coffee filter before I let things cool down and boy that coffee filter looks nasty. I've no idea how much of that nasty is really from the alks or from the added salt itself, I don't care actually I just get rid of it.

It doesn't seem to ruin the yield (around 2% from rue)

That is low, I always get at least 5% freebase and last time 8% freebase. Maybe you have bunk seed or lost in extraction or combination? And yes grinding is not necessary as my yield illustrate.
I don't know the GordoTEK, it's not in the forum wiki nor on Gordo's youtube channel, maybe I missed it somewhere? Anyway it can't be ineffective I suppose.
Luckily te seeds are cheap so not a big deal, but I'm sure you can raise your yield if only for the sport of it :thumb_up:

Happy trials.

 

[murklan]

... I always get at least 5% freebase and last time 8% freebase. Maybe you have bunk seed or lost in extraction or combination? And yes grinding is not necessary as my yield illustrate...

Have you written down the way you are doing the Rue extraction Jees?

 

[Rolinwama]

Hi Rolinwama,
great you are playing with possibilities :thumb_up:

...In all the guides it is said you have to go through this freebasing/salt crystallization few times (like 5 or so) to have the product purified.

A few manskes gives me a nicier yellow product indeed but some people are convinced that just 1 manske is really enough in terms of ridding the quinazolines effectively, so there is not 1 take on this. Since I do several A/B transitions (with filtering the acid stage) the alks are fairly clean and 1 manske suffice nowadays.

The trick I have found out is that during the salting step, keep the solution in a hot (near boling/boling) water bath and add as much salt as possible (if there are leftover grains it won't be a problem) - just saturate the hell out of the solution with salt. Now the most important part: keep the solution in the hot water bath and wait.

What will happen after 30-40 minutes if you keep the solution hot: the salt form harmalas will remain dissolved in the solution (keeping in hot water bath will prevent harmala salt crystallization), yet the gunk will precipitate out!

I also find gunk in the salted liquid (even when heading for 20gr salt/100gr liquid) , therefore I poor the very hot salt liquid trough a coffee filter before I let things cool down and boy that coffee filter looks nasty. I've no idea how much of that nasty is really from the alks or from the added salt itself, I don't care actually I just get rid of it.

It doesn't seem to ruin the yield (around 2% from rue)

That is low, I always get at least 5% freebase and last time 8% freebase. Maybe you have bunk seed or lost in extraction or combination? And yes grinding is not necessary as my yield illustrate.
I don't know the GordoTEK, it's not in the forum wiki nor on Gordo's youtube channel, maybe I missed it somewhere? Anyway it can't be ineffective I suppose.
Luckily te seeds are cheap so not a big deal, but I'm sure you can raise your yield if only for the sport of it :thumb_up:

Happy trials.

Some of the gunk is definitely alks, the solution is a lot clearer after this "degunking" than it was before the salt was added.

And yes I think the rue I had was low on harmalas and also my impatience. 2% yield is good enough for me given the speed of the process with trick in the OP.

 

[Jees]

...Have you written down the way you are doing the Rue extraction Jees?

Not really. I think 3 factors play for yield:

(last time I froze/thew a few times the wet pH3 soaking seeds as a prelude)

1) seeds potency:
not much to say about this

2) the boiling stage:
I change water 4 to 5 times on the seeds, but each of those washes gets like 4 times sequentially a boil in the pressure cooker. The 4x pressure-on then pressure-off should (in my imagination) seep water in and out of the seeds. Water is 3 to 4 pH citric acid added. Pressure-off is enough, no need to cool down before pressure-on again. Each pressure-on stage is like boiling for 2 hours.
For 150 gr seeds a wash volume is like 1.5 liter water.

3) A/B + maybe manske.
try not to loose alks here, by upping pH enough to at least 11 better 12. Dissolved lye is used for adding base. For Manske I've found 20gr salt/100 gr liquid enough.


So nothing really magical

 

[Rolinwama]

...Have you written down the way you are doing the Rue extraction Jees?

Not really. I think 3 factors play for yield:

(last time I froze/thew a few times the wet pH3 soaking seeds as a prelude)

1) seeds potency:
not much to say about this

2) the boiling stage:
I change water 4 to 5 times on the seeds, but each of those washes gets like 4 times sequentially a boil in the pressure cooker. The 4x pressure-on then pressure-off should (in my imagination) seep water in and out of the seeds. Water is 3 to 4 pH citric acid added. Pressure-off is enough, no need to cool down before pressure-on again. Each pressure-on stage is like boiling for 2 hours.
For 150 gr seeds a wash volume is like 1.5 liter water.

3) A/B + maybe manske.
try not to loose alks here, by upping pH enough to at least 11 better 12. Dissolved lye is used for adding base. For Manske I've found 20gr salt/100 gr liquid enough.


So nothing really magical

Interesting, I am doing 3 PC cycles 3 hours each with water changed once per cycle, you are doing way more and maybe this is the reason you get better yields (perhaps most harmalas are still trapped within seeds for me.

Regarding ph of 11-12 does it really make a difference from the usual 9.8 or so?

 

[murklan]

...
So nothing really magical

Thank you! I've never used a pressure cooker for this. Mainly because the one I have wont work on my induction stove. And the times, if I understand, are 2h pressure-on x 4 and then changing water 4-5 times. That is 4 x 2 x 4-5 ... that is quite some time

I usually do 50g at a time but If I would do it your way I surely would make more while I'm at it. Next time!

 

[Jees]

I'm sure doing an overkill. Sometimes it takes a week or 14 days, sometimes 2 days nothing happens then I continue, or doing just one boil on a day, it's like there is a friend in da house :lol:
What also takes time is each base phase is settled one day before I skim off[***] the top layer to discard, I've never have hard filtrations problems.

[***] I made a 'sucker' for taking the base top layer off the bottom alks, I don't tilt over the pot like decanting bc it disturbs the bottom layer. See attachment here. In that post I use the sucker to remove a wash out of the pressure cooker seeds, the seeds don't leave the pot for convenience only, an easy lazy workflow.

@ Rolinwama: I'll make a comparison between pH 10 or 12, I hope tomorrow.

 

[downwardsfromzero]

Jees - are your PC boils literally bring it to boiling at pressure, followed by removing the heat and leaving a while to depressurise? Or do you have a preferred duration for the PC boil?

 

[Jees]

Jees - are your PC boils literally bring it to boiling at pressure, followed by removing the heat and leaving a while to depressurise? Or do you have a preferred duration for the PC boil?

Both happen as much. The ramp up and swift down is the practical choice if one prefers to minimize a kitchen hostage time. Cant tell if a 1 hour boils stage yields more, but I do it anyway as default {max timer setting}.
One could also choose between
* reboil start as soon as pressure is off, still hot though
* reboil start as soon it cooled to room temp

I haven't made comparisons really, because it's not in my living spaces I deviate from a pattern-for-a reason. When I pass that pot I say 'hey dude what you wanna do?' then sometimes I feel to give it a stage of contemplation, why not a day? Perfectly possible Sir. Or I sense it wants to get on-business, so there goes any consistency on my part. If it was in my private kitchen I'd opt for fastest process i.e. short max-press-stage and short pressure-off-stage. Less time available? --> Less cycles can help too. White coat unworthy, I never write or log yields and ever changing hands-ons.

 

[downwardsfromzero]

[...]

I haven't made comparisons really, because it's not in my living spaces I deviate from a pattern-for-a reason. When I pass that pot I say 'hey dude what you wanna do?' then sometimes I feel to give it a stage of contemplation, why not a day? Perfectly possible Sir. Or I sense it wants to get on-business, so there goes any consistency on my part. If it was in my private kitchen I'd opt for fastest process i.e. short max-press-stage and short pressure-off-stage. Less time available? --> Less cycles can help too. White coat unworthy, I never write or log yields and ever changing hands-ons.

Thanks for the clarification. Sounds like we have an uncannily similar approach to the workflow :lol: