[Work Space] No filter, No reduce Syrian Rue Extraction

[pitubo]

By all means manske if you feel compelled to. Honestly I don't know enough about harmala alks generally to give them to a pregnant woman in the first place, regardless of vasicine.

It's not just about pregnant women, it's about women in general who may experience uterine discomfort due to the quinazolines.

But as far as what we do know:

content of dried plant material for the other alks:

Vasicine (peganine) - 0.25%
Vasicinone - 0.0007%

That study also lists:
Harmine - 0.44%
Harmaline - 0.096%
Which makes the vasicine content anything but negligible. An extract with such composition would contain about 1/3 vasicine by weight!

according to:
Pulpati H, Biradar YS, Rajani M (2008). "High-performance thin-layer chromatography densitometric method for the quantification of harmine, harmaline, vasicine, and vasicinone in Peganum harmala". J AOAC Int 91 (5): 1179–85. PMID 18980138.

There are several studies to be found. The problem with some of these studies, such as the above mentioned, is the use of anhydrous methanol for the initial extract, upon which all further analysis is based. Obviously, less than 0.5% yield of betacarbolines is unusual and unexpected in the light of the results on the nexus and in this thread. Another study that used 1:1 methanol/dilute HCl for initial extraction found results more in line with yields reported here.

Plus from personal experience and many other trials reported among rue extractors, basing leftover manske water recovers an extremely small amount of precipitate, which may contain a lot of harmala. I think there was even a lab test of this residue and it was determined to be mostly harmalas, but I might be misremembering. Does anyone recall this? At any rate, the amount of vasicine is very small.

AFAICS the data is mostly lacking. Even scientific studies seem to have trouble getting the procedures right. Did the person who prepared the samples for analysis in that thread use sufficient base when basing the manske filtrate? In my experience, when throwing in a boatload of lye, I got quite a bit of precipitate. This, when redissolved into a significantly smaller amount of acidified water, still yielded little harmala needles from re-manske.

 

[ouro]

Like I said previously, everyone should do their own research before eating anything... I am not trying to convince anyone to eat or make general policy regarding eating non mansked rue extract.

For completeness:

here is the record of Snozzleberry and endlessness lab tests on the manske residue: Vasicinone, Vasicine and Deoxyvasicine - Collaborative Research Project - Welcome to the DMT-Nexus

I'm not a trained ayurvedic herbalist, but I don't see any caution for women to use justicia adhatoda beyond the pregnancy abortion warning.

Regardless, this thread is not intended to be a discourse on vasicine. The practical take away is that you can wash your crude harmala precip with water and it will contain some vasicine, and based on the evidence we have it is probably a very small amount. If this concerns you, you can continue to do a manske.

 

[pitubo]

Regardless, this thread is not intended to be a discourse on vasicine.

Agreed, the research in this thread is interesting and useful.

The practical take away is that you can wash your crude harmala precip with water and it will contain some vasicine, and based on the evidence we have it is probably a very small amount.

This I don't agree with. IMHO the evidence we have is rather scant. Look at the study that you quoted earlier - it would imply 1/3 of the extract is vasicine, and 150 mg of freebase would contain only 100 mg harmalas.

So apart from any potential issues with vasicine, which may be less to the point here, there's also an issue with the exactness of dosage. One simple manske step would eliminate almost all of the quinazolines and thereby also the dosage reliability issues.

I really like the simplifications that this thread proposes, but skipping the manske is IMHO cutting a corner too much.

 

[brilliantlydim]

So I took 200g of Syrian Rue seeds

1.Added water to cover them and freeze thawed a couple times
2.Added 2L of water and some vinegar boiled for 1 hour
3.strained out seeds, kept tea
4.Repeated step 2 and 3 with fresh water
5. Combined boils
6. added Lye until colour stopped changing
7. let sit until most solids precipitated
8. Decant as much of the liquid as possible
9. added fresh water
10. repeated 8 and 9 about 8 times until water was pretty clear and ph was the same as water I was washing with
11. decanted, put sediment in baking tray and put in the oven on lowest setting until dry
12. scraped
13. smoked

I got about 4.5g which is low yield, but for the cost of the seeds, the amount I smoke and amount of work I did it didn't seem too bad. Its probably a few years supply fro me. Not the purest extract tek, but smoked nice enough.

I did save the seeds, so I figure I can do some more boils and extracts on them when I need more.

Next stop, making some changa

 

[downwardsfromzero]

And here's a bit about vasicine:

http://iglobaljournal.com/wp-content/uploads/2011/02/RACHANA-ET-AL-9.pdf

 

[DeeMenTalist]

My try of this 'tek'.
Briefly what I did.
One freeze/thaw 200g of seeds.
4 boils in acidic water about 40-50mins each.
Filtered seeds> based solution> let it precip> decanted> washed each boil 3 times.
combined all and then washed again 5 times.
So I ended up with 9.8g of this goodness. I`m sure there was more but I need to get some better filter. I lost some amount during filtering process.

 

[eastlancsguy]

Sorry to raise an old topic from the dead, but I can't find this info anywhere....

Could this same technique be used to extract Harmalas from B. Caapi leaves?

 

[Kerberos]

My try of this with 250g (big mistake i know, but i got 2Kg from our sponsor so thought why not!)

1. Boiled for 1 hour with 2l of water and Phosphoric acid which took the ph down to 2
2. sieved brew into 1l kilner jar and based. Did this 3 times.
3. Added cold water and a dash of Phosphoric acid to the pan and left over night as i ran out of time.
4. Next day boiled for an hour and based, did one more pull to make 5.
5. Attached image shows the first 3 pulls in jars 1 and 2, third jar is overnight pull 4 and final jar is pull 5. They have all had several rinses to bring the ph down, 4th pull is taking longer than the others to settle out which is why it still looks dark.

6. Acidified with phosphoric acid and let settle.
7. siphoned off liquid and used my aeropress to filter the liquid.
8. Based this.
9. There was a lot of "sediment" left so i added more water and acidified this.
10. siphoned, filtered and based this second pull and as there was some precipitation i repeated acidifying the sediment that was left.
The following image show pulls 1 and 2 and the acid solution waiting for me to see if there are any more goodies in this.

I will post some more pics when i have done the third pull and left everything to settle.
I also have a jar acidified with vinegar so i can compare the Acetic acid and the Phosphoric acid and will post pictures of those pulls also.

 

[Lichen]

My try of this with 250g (big mistake i know, but i got 2Kg from our sponsor so thought why not!)

I've only just begun looking into syrian rue extractions, why was using 250gm a big mistake? Is it just better to use smaller amounts?

 

[Kerberos]

My try of this with 250g (big mistake i know, but i got 2Kg from our sponsor so thought why not!)

I've only just begun looking into syrian rue extractions, why was using 250gm a big mistake? Is it just better to use smaller amounts?

Yeah small amounts, i am using 7 jars at the moment! Next time i would only do 50g,i say next time but i think i am going to have enough to last a life time from this extraction.:d

 

[Lichen]

I'm going to attempt this this extraction soon but have some questions? How much does temperature play a role? When I add base to my tea, does it need to be at a certain temperature? Cool? Chilled? Straight off the stove? Does it matter?

Also, surely there must still be some sort of filtering required - after brewing the tea and straining the seeds out, I imagine there must still be particles all through the tea that would require filtering out?

 

[roninsina]

Hi Lichen, I just used this method for my first successful rue extraction. I put 100g with water, in the microwave and brought to a a boil, then on the stove for an hour, let it set on the stove overnight with lid and no heat. Brought it to boil the next day and strained the tea through a wire mesh sieve. Then repeated this four successive times (I'm sure there are more efficient ways to extract the tea but I didn't have to spent a lot of contiguous dedicated time.) with fresh water.

I based the cold tea with lye solution (it gets hot when you add strong base) and let it settle for several hours. I siphoned off the non-solids with a turkey baster and added fresh water 7 times.

Then I salted the solids with vinegar so they were now in solution. I let that settle for several hours, and could decant my solution to another container, as the residual plant matter stayed on the bottom.

I chose to do the Manske at this point as I'd be gifting a significant portion of the yield to others. I may skip it if I get to a batch that's just for me. Another reason I mention the Manske is because I did put the hcl crystals through a coffee filter at this point and it took all of about 30 seconds.

I dumped the hcl crystals back in my jar and rinsed the filter with hot sodium carbonate solution as I filled the jar back up with the same solution. It's back to the waiting game of settling again, and these take a long time to settle if you use sodium carbonate, as the particles are very fine. I siphoned off the cleared water (leaving the free-base harmalas at the bottom with a small amount of the ever weakening base solution) and added fresh water 6 more times.

I put this in a large baking dish to dry at low temp in the oven, and scraped up the goods a few hours later. Very pale and potent.

Thank you so much to all the folks who've contributed to the evolution of this process. And a special thanks to Intezam, as I have chronic back pain that is mitigated by harmalas - I might have never known.

 

[Lichen]

Ok, I think I'm beginning to understand that the process of basing and decanting, and acidifying and decanting is a big part of the separation of harmala alkaloids from unwanted gunk and plant matter.

"Discard all solids when your material is acidified, and discard all fluids when it is based" - I now understand that this is literally a form of filtration/separation.

Regarding the manske:
I'm with Pitubo on this - skipping the manske is cutting a corner too much, and would rectify any dosage issues and any possible uterine discomfort from the quinazolines.

Question is however, should I redissolve the harmala hcl crystals after the manske, and basify (and wash and evap) once again to store as freebase, in order to avoid salt contamination, and dosage issues?

 

[roninsina]

^^^^^^^
Sorry if I added to the confusion, with my omission of details, Lichen. You may want to wait for a more experienced member to chime in, but what you suggest, worked for me. After the Manske, I filtered the hcl needles through a coffee filter to get rid of most of the saline. Then I dissolved them in 1 cup/250 ml of hot water. Then I added a couple of teaspoons of sodium carbonate to the harmala hcl solution, which started some of the precipitation of free-based harmalas. I then heated a separate vessel with 1 cup/250 ml of water, and added (while stirring) sodium carbonate until it was saturated and there was some residual on the bottom - even after some stirring. I then added this saturated sodium carbonate solution to the harmala solution and stirred. It takes a few hours to fully settle and then you can decant/siphon off the sodium carbonate solution from the precipitated free-based harmalas at the bottom. You can now fill your vessel back up with fresh water and stir it, let it settle, decant/siphon again, and repeat this step until you feel you've washed out enough of the sodium carbonate (I did it a total of six times). Then the harmalas are ready for drying.

 

[pitubo]

Question is however, should I redissolve the harmala hcl crystals after the manske, and basify (and wash and evap) once again to store as freebase, in order to avoid salt contamination, and dosage issues?

To minimize the salt residue in harmala HCl crystals, there are five techniques that I am aware of:

1. Let the hot saline harmala solution cool very slowly. This gives large needle crystals. More bulky crystals have proportionally less surface to which saline solution can adhere while drying.
2. Do not use more than 10% salt.
3. Vacuum filtration on a buchner funnel. After most liquid has been pulled through, the airflow will suck out some of the saline liquid stuck between the crystals.
4. If you value purity over yield, give the crystals that have collected on the filter a last rinse with a small amount of ice cold water. This works best in combination with vacuum filtration, to quickly suck off the water before substantial amounts of crystals dissolve again.
5. Press the filter cake between many layers of kitchen paper. Refresh the kitchen paper once it has become wet and press again until no more liquid seeps into the paper.

 

[Terrence_Mechanic]

Is Arm and Hammer Washing Soda Ok and safe to use?

 

[pitubo]

Is Arm and Hammer Washing Soda Ok and safe to use?

Probably, yes. Swimming pool "pH up" should also be okay.

 

[roninsina]

Is Arm and Hammer Washing Soda Ok and safe to use?

Probably, yes. Swimming pool "pH up" should also be okay.

That's what I used. [Edit: I used Arm & Hammer Super Washing Soda] I searched several sites and the msds, and all said 85% sodium carbonate and 15% water. If there is anything else in there, it's water soluble as far as I could tell. Unless there is something pretty bad in there, the water washes should dilute it beyond concern.

 

[rootBarkEnthusiast]

This is my first successful harmala extraction, so I don't have much to compare this with. But I had a pretty easy time with this. I only used 30-40g of rue for this, and I did a manske just for fun but in the future I'll probably just base 100-150g of tea and wash it.

Here is what I did in detail:

First I made the tea, after covering the seeds in vinegar, soak, and freezing/thawing, I boiled them in a large pot for about an hour before straining the tea into a smaller pot, basing that, and adding more water to the big pot.

After basing a pull of tea, it took a few minutes to settle for me to decant the base water, and I was able to have it washed by the time the next pull was ready.

After 3 pulls I decided I wanted to try a manske because some of the hcl crystals ive seen on here are pretty. I think I lost some of the goods in this step, but here is the result.

I have not tried the harmala hcl yet, but I have tasted on my fingers after handling and its extremely bitter.

 

[rootBarkEnthusiast]

lets see if we can figure out pictures.... Also I used NaOH for a base