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Ethyl Acetate Approach for Harmala Options
 
_Trip_
#1 Posted : 8/30/2021 6:47:54 AM

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Note Some photos from my posts have been removed due to the host website being down.**** Some photos have been recovered and newer photos will be added later down the track.
Lab results Page 3

Hi Nexians,
I have currently been experimenting with CIELO Tek for mescaline with great results. Anyway after being inspired by this Tek I experimented and gave it ago for harmala extraction of Syrian Rue seeds with a few mods. The idea is for a fast and pure tek.

The process was rushed and little measurements were taken. It was more a proof of concept.
Bottom line it appears successful. See photos below.

-Dried Syrian Rue seeds were blended up into a powder. 66g in total.
-200ml of water was added to 16g of calcium hydroxide (pickling lime) and mixed.
-The ground up rue seeds where added.
-This was placed in the microwave and put on for short bursts of 3 mins (750 watts) and mixed in-between. Until two thirds of the water content (the 200mml) was evaporated.
-This was cooled and ice cold ethyl acetate was added (100mls) x4 pulls. (1min each pull).
-The ethyl acetate pulls were decanted off with a french press.
-The combined ethyl acetate was filter with a lab filter and vacuum pump
-10g of citric acid was added and shaken vigorously. It was not left for more than 15 minutes.
-Orange crystal like structures formed quickly, when i say crystals more like clumped half melted sugar.
-about 5g of NaCl was added (don't ask me why i was just experimenting)
-This clumped at the bottom and stuck to the side of the walls of the jar.
-Ethyl acetate was decanted.
-Hot water and vinegar was added to the NaCl and citric acid and dissolved.
-This was then based with sodium carbonate and shaken. Eventually the solution cleared up and Harmala formed and floated to the top.
-After letting this cool it sank to the bottom of the jar.
This whole process was actually completed quite quickly and with little mess.

Current Yield: 1.24% (light tan color)
Edit: 3.7%+ with potential to yield more
Edit 2: 4.9%+ with potential to yield a little more

Every acid and water wash was attempted on the left over EA (which was split up) but nothing much seemed to precipitate. H2O washes were performed, acid washes with vinegar, fumaric acid was tested, NaCl, more citric acid and then eventually all experimented washes were based with sodium carbonate, minimal ammounts precipitated. The citric acid one precipitated a bit more meaning maybe more citric acid should be added next time maybe up it and try 20mg/gram in the ethyl acetate. These will be left for 24hrs and reported back on.


I am still yet to experiment with pulling more from the Rue seeds. More ethyl acetate and warmer pulls may facilitate a better result. So my reported yield may well increase, 4 cold pulls over 4 minutes were likely not enough.

If one was hoping for 4-6% pull from 66g of rue seeds then 2.64g-3.96g would be ideal numbers. Although my initial pull did not yield this there is plenty of room for improvement to get these numbers up.

I still need to figure you what helped the harmala crash, citric acid, NaCl or both? This will be experimented with next. I would think it is the citric acid. Since I have no chemistry background its more or less a crude trial and error.

Thanks to Loveall and everyone who worked on the cielo Tek. If yields can be increased this harmala extraction may prove to be a quick easy and less messy alternative.


_______________________________________________________________________________________________
Edit:
For those that can't be bothered reading this thread and want to give this Tek a go. Although there's still ongoing experimenting the current Tek (to get decent yields and decent looking purity) stands here:
Tek can be done in 2.5 hours maybe quicker.
This process could change and will continue to be updated.


Step 1:
-Add 300ml of water to 25g of calcium hydroxide and mix to form 'base water'.
Alternatively one can use sodium carbonate (this may negate the need for filtering later).

Step 2
-Get 100g of dried ground up rue seeds and mix with 'base water'.

Step 3
-Microwave the rue/base mix until 2/3rd's of the water content is steamed off (use kitchen scales to measure this). As a guide a 750 watt microwave at 5-7min bursts should work fine. Mix between bursts. Several burst will be required.

Step 4
-Prepare a warm water bath with boiling water and warm 1lt of EA. No open flames.

Step 5
-Conduct 6 pulls with the 1lt of EA. So 160ml approx per pull (keep in mind rue seeds will absorb a little bit of EA).
-Using a french press do 6x pulls from the rue seeds (6 warm pulls at 1-2 mins each). Decant from the french press after each pull. Keep rue base mix and EA in the warm water bath to improve yield (obviously in their respective glass jar/ french press).

Step 6
-Approx just over 800ml of EA should be recovered and then filtered (filtering may not be necessary if one has used sodium carbonate as a base). Lab filter is recommended, coffee filters should work too.

Step 6a (optional)
-To increase purity one can chemically dry with CaCl2. The citrate in step 7 will not be a goo but a crystal like formation instead. (This step still requires further investigating as end product may still be the same appearance in purity).

Step 7
-Add 16g of citirc acid to the combined EA and shake for 5-10mins (red/orange/yellow oil should form). Orange/red goo forms at the base of the jar and the rest of the jar gets covered with sticky yellow goo (making it easy to decant). (This goo should crystalize if left for 24hours+. This is not necessary though one can decant right away).

Step 8
-Decanted EA. (this can be cleaned and reused next extraction). One can also add a little bit of EA to the citrate stuck to the jar to clean it up a little bit. Again decant this EA.

Step 9
-Add 600-850ml of warm distilled water to the citrate goo, it will dissolve fairly quickly. 300-400ml may suffice. (Ratio it down if using less seeds). The more water the more sodium carbonate may be needed depending on yield but the more water used gives a cleaner product.

Step 10
-Base slowly with sodium carbonate (shake once acid is neutralized).

Step 11
-Harmala will crash out quickly. Some of the FB harmala will float to the top, this needs to be left to cool.
(Sticking the jar in a freezer will speed up the process and the floating harmala should settle. This should not take long). Once it has finished crashing out filter and dry the product. No need to leave this overnight, if left for too long (say 24hrs+) some impurities may crash out. The final product in this step should crash out quick and should/ can be filtered within a hour or 2 (often quicker).As a rule of thumb I wait for the floating harmala to settle to the bottom this is rarely exceeds the 2 hour mark.
Once filtered and dried you have the final product.

Note: One could carefully decant but some product will be lost.

Step 11a
-This is optional but a mini EA A/B can be done on the final product to clean it up. This may not be necessary but is recommended if the final product comes out as a dark tan instead of a much much lighter grey/tan color. If each step is followed it should come out very very clean to the naked eye anyway.
-Dissolve the final yield in 50ml of warm EA or add a little more EA until all FB harmala is dissolved. Crash it out again with citric acid, decant, add distilled water, base and crash with sodium carbonate, separate/filter and dry again.

This should yield approx 3.7% first run. (See photos on the below and on second and third page).

One can repeat the whole process again to increase yield to over 5%+ (recycle and cleaning the used decanted EA works fine).

Disclaimer: All my posts are of total fiction.



 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
Loveall
#2 Posted : 8/30/2021 8:59:43 AM

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Very cool, looks promising.

I'm going to try to repeat. Since yield was low, will do couple modifications on what you did, see if we learn with another data turn.

- Base after microwave: Reason is that FB harmalas are not soluble in water (unlike FB mescaline), this may help get the harmalas out of the plant matter so the quick EA pulls work better (not sure).
- Try room temp pulls: Harmala FB are tough to dissolve in solvents, maybe chilled EA is not pulling enough and why your yield suffered, not sure. According to the attached paper, ethyl acetate is a good choice in A/B extraction (so I think you are indeed onto something). Perhaps using pH paper like we did during CIELO development may help track how well the pulls are going (want pH paper in EA to go from basic to neutral after only 4 to 5 pulls).
- Chemichally dry EA with washing soda before salting: This may not help with anything, but is a good thing to do just in case the ~5% water in EA is causing any issues. It is not a lot of work and makes the process more aligned with standard lab practices (e.g. attached paper). I will not add NaCl to the EA, in your case it may have attracted a little water and clumped up,not sure.
- I'll wash any xtals that crash with fresh EA, see if any off colors are removed.

I'll report back with results. Thanks for the idea and testing it out _Trip_ 🙂

Note: Harmalol may go into EA if baking soda is used as base (since it will be near its isoelectric point). This could be a path to recover it, instead of dumping it during the first alkaline water precipitation.
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_Trip_
#3 Posted : 8/30/2021 9:18:03 AM

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The idea of basing before microwaving was more to facilitate mixing of the base and keeping water content low. But your right as FB harmala isn't water soluble it wont matter if it was based afterwards as water shouldn't be an issue and can be chemical dried with Cacl2 later. So the idea of microwaving first then would be to lyse cells in a little bit of water?

And I agree on room temp, I still have my 66g of rue seeds I will attempt to heat the ethyl acetate in a warm water bath and then try a few pulls see if i can yield a bit more (i do have strips).

I was wondering if a larger range of beta-carboline alkaloids would survive this process or could if the tek was modified.

Definitely keen to see what you come up with Loveall.

Keep us posted.
Disclaimer: All my posts are of total fiction.



 
Loveall
#4 Posted : 8/30/2021 9:46:52 AM

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The first water/microwave step would be to "shake" loose harmalas from a complex plant matrix on/in the seeds into a simple soluble form in water. Avoiding the early basing is so harmalas remain soluble (aka so that water has low chemical potential from the harmala point of view). This way, harmalas will have an incentive to leave the plant matrix. I could be very wrong though, just got to try the experiment.

This is not as much of a concern for mescaline because it is somewhat soluble in alkaline water.
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_Trip_
#5 Posted : 8/30/2021 10:15:06 AM

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I get ya.

Cheers Loveall just trying to gain a better understanding.

I tried warm pulls will report back soon. Going to try citric acid only this time no NaCl.

Edit: That 1.24% yield will increase, i did some warmer pulls and managed to get more out of it. It's cooling and precipitating now. It looks a bit cleaner in the solution than the last run maybe you're right and the NaCl added contaminants by pulling in EA or what little water was present.

I used strips and still believe there's more to pull from the original 66g. Note* I did 4 more pulls again with warmed EA (and the EA was recycled from the last run). H2O washes followed by a sodium carbonate wash 35% water weight as per cielo tek. So it looks like we an definitely reuse EA here as well.
Edit: Forgot to mention CaCl2 was also used to dry the reused solvent before the second run.

Bottom line warmer pulls and citric acid only might be the go.

I don't want to speak too soon but i think there's been a massive increase in yield over the first run. Also when you dump the citric acid in, and it goes an orange like goo it must be dense with harmala citrate because it doesn't look like much until you add vinegar and water and then base to precipitate.
Disclaimer: All my posts are of total fiction.



 
Loveall
#6 Posted : 8/30/2021 4:15:15 PM

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Thanks _Trip_

I gave this a go:

Microwaved 50g of rue seeds in 150g of water (whole seeds, because I'm lazy and wanted to see what happened). After evaporating 40g of water with a few runs with stirring, the moist seeds had absorbed almost all the free flowing water and looked ready for a "dry tek" pull. At this point I added 12.5g of washing soda, and the seeds released a bunch of water, so I microwaved more, and after 40 more grams of water where evaporated, the mix was again moist with almost no free flowing water (once again, it looked ready for a "dry Tek" pull).

While this mix was still hot from the microwave, I covered it with ethyl acetate + two fingers. The wet seeds where so hot that the solvent boiled for a couple seconds (ooops). I stirred for a few minutes and tested the solvent with pH paper: got deep green consistent with pulling alkaloids right away.

The EA was decanted, chemichally dried with washing soda (unknown if this is needed, but could be a good standard practice), resulting in 85g of orange extract (first image). Adding 200mg of citric acid resulted in massive white clouds, confirming _Trip_'s result that something interesting is coming through. pH paper was still green after 200mg of citric, so I added more citric acid until the pH paper was no longer green. The solution became milky throughout when acidified (second image) with am orange residue settling at the bottom. Looks like sticky orange xtals/goo are crashing which could contain the product (and possibly other stuff?).

Started a second pull at room temperature. After 5 minutes it didn't look like much was being pulled as the pH paper barely changed color to a very light green. After 30 minutes, the pH paper looked a little darker, so I'm letting this second room temp pull rest/soak until the pH paper color stops darkening (an indication that it has reached equilibrium). 3rd picture has the 3 pH paper measurements during the pulls (one from the first pull and two from the second pull).
Loveall attached the following image(s):
IMG_20210830_103031793.jpg (674kb) downloaded 595 time(s).
IMG_20210830_105946892.jpg (533kb) downloaded 593 time(s).
IMG_20210830_103841446.jpg (625kb) downloaded 592 time(s).
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_Trip_
#7 Posted : 8/31/2021 2:41:13 AM

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Looking good Loveall, have you tried to FB the goo?

So after doing a second (warmer) pull from my original 66g of rue my final yield is now sitting at 3.7%. Big grin

Second time i did 4 warm pulls of EA this was filtered (it was not chemically dried) and then citirc acid was dropped just under 20mg/g. It was shaken for 10 mins. EA was decanted and the orange goo was collected.
With a 1:3 hot vinegar to warm water mix at (250ml) this was added and then shaken to dissolve the goo. It was then based slowly with sodium carbonate and again harmala formed. The harmala was then filtered and left dried. It yielded double the cold pulls.
Note as it is already in a acid form vinegar may be unnecessary.

It still believe if i mash the seeds a little bit and do another 4 or more warmer pulls with the EA that my final yield will increase again. I'm going to wash the goo a bit better next run with clean EA to see if I get a cleaner looking Harmala product. Having said that it appears fairly clean anyway and is a off tan color not a dirty tan.

With the percentages now recovered I think this has potential to be a good Tek.

Also the EA that was decanted from the second pull was left in it's own jar over night interesting more harmala citrate formed (rather I should say what appears to be harmala citrate since its untested). And incredibly some crystals actually formed. I now believe like the cielo tek, that maybe if less citrate is used and left overnight crystals may form instead of a goo. (see last photo)


I think if i start from scratch again I'll need to take better measurements like you have Loveall. And without testing who knows exactly what is being pulled and crashed out but I think it has potential.

Since basing first seems to be working for me I may do that again first. In the meantime when i have a spare minute I'll try to squeeze a bit more from my original 66g.

The yield will go up to over 4% with another couple warm pulls from the original 66g and from the left over EA from the second run (warm pull) which crashed out more harmala citrate over night. So I can confidently say yields for this tek can reach over 4%.


EA after pulling from the Rue and Calcium Hydroxide mix


After filtering


After adding citric acid


After shaking the citric acid mix (it forms the orange goo)


After decanting EA and dissolving the orange goo in vinegar/ warm water and then basing with sodium carbonate. You can just see it precipitating.


Result after it is left to cool



End result once dried


Results after the decanted EA was left over night (second run warm pulls). More Harmala citrate crashed out. it left a ring of orange goo around some crystals (very interesting).
Disclaimer: All my posts are of total fiction.



 
Loveall
#8 Posted : 8/31/2021 3:34:25 PM

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Very interesting, I haven't based my orange goo yet (looks exactly like yours).

Looking at your water basing step, looks like the orange/yellow color ends up in the water? I think this is unwanted stuff that may be stopping xtals from forming during the first precipitation with citric.

Your product looks very whit to me.

I wonder what would happen if you dissolved your freebase dry harmala candidate in EA, and added citric. Do you get xtals or a goo again? I'll try this when I get a chance.

The strong temperature dependence you have found is interesting. A couple other things that may be worth trying:

1) Put the warm EA pull in the freezer. Ice water will float at the top. Does harmala FB form at the bottom? If yes, that would be really cool. Harmala FB are difficult to dissolve so I wouldn't be terribly surprised if this worked. If nothing crashes, adding Naphtha may cause FB harmala candidate precipitation, but downside is that re-using solvent for another extraction.
2) The orange color appears soluble in water based on your picture where FB harmalas are crashing. Perhaps washing EA from the pulls with brine or washing-soda-saturated-water removes the color in EA. Maybe adding citric acid to the washed EA forms xtals instead of goo?

Also, I have realized that I did not fully dry my first EA pull using washing soda. I used CaCl2 to dry my second pull and that removed a lot more water, also some orange stuff crashed when the water was thoroughly chemichally removed. I'll report back on what crashes out of this when adding citric acid.

This is so much fun 🙂
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Loveall
#9 Posted : 8/31/2021 7:46:59 PM

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Loveall wrote:
1) Put the warm EA pull in the freezer. Ice water will float at the top. Does harmala FB form at the bottom? If yes, that would be really cool. Harmala FB are difficult to dissolve so I wouldn't be terribly surprised if this worked. If nothing crashes, adding Naphtha may cause FB harmala candidate precipitation, but downside is that re-using solvent for another extraction.
2)The orange color appears soluble in water based on your picture where FB harmalas are crashing. Perhaps washing EA from the pulls with brine or washing-soda-saturated-water removes the color in EA. Maybe adding citric acid to the washed EA forms xtals instead of goo?

Also, I have realized that I did not fully dry my first EA pull using washing soda. I used CaCl2 to dry my second pull and that removed a lot more water, also some orange stuff crashed when the water was thoroughly chemichally removed. I'll report back on what crashes out of this when adding citric acid.


Alright, been a busy morning. Some results.

1) Tried this and only saw floating ice, no FB forming at the bottom 👎
2) I washed a pull with water 3 times. Doesn't work, still got oil when adding citric 👎. However, I reserved a portion of the washed solvent and salted with Fumaric acid. That is giving a yellow/brown precipitate that is xtaline. Will report back on how it looks after decanting.

Other experimental updates:

3) The fully dried extract with CaCl2 is interesting. A bunch of yellow stuff crashes when the water is removed and can be seen between the white CaCl2 pellets (see image below). Nothing crashes out of the dry solvent when salting with citric (?) but perhaps I was impatient. Salting with Fumaric did crash white xtals quicky. Dissolving the organic acid is a lot slower in dry EA. Perhaps harmala citrates like to form with water and that is why they are oily in the raw wet extract and not showing up quickly in the dried extract. Fumaric acid does not seem to have this issue. However, the citrate oil is great for decanting and is perfectly fine since for a quick FB conversion in water.

4) The 3rd pull on whole seeds with EA kept on pulling with time: pH paper kept on getting greener for about a day. Looks like the pulls from whole seed take time (but work) and need to be warm (unlike with cactus where they are very fast and cam be done very cold).

Random comments/thoughts:

The process of getting harmala FB out of seeds with EA reminds me of whole coffee bean decaffeination where steamed coffee beans are soaked for 8+ hours in EA (caffeine is in FB form naturally so no base is required). This long soak seems beneficial for rue seeds (unlike the cacti paste where mescaline extraction is very quick and a long soak causes congealing issues).

Finally, the paper in post #2 claims that harmaline can be pulled with EA when basing with sodium bicarbonate. That is surprising, but also interesting. Harmalol my also be pulled under those conditions and could also precipitate when salting 🤞
Loveall attached the following image(s):
IMG_20210831_142552802.jpg (651kb) downloaded 507 time(s).
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_Trip_
#10 Posted : 8/31/2021 11:11:15 PM

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I just put in an edit that I forgot to mention when I cleaned the reused EA for the second warmer pulls i did use CaCl2 to dry it. The color stayed yellow the caCl2 stayed white.

Loveall wrote:

Looking at your water basing step, looks like the orange/yellow color ends up in the water? I think this is unwanted stuff that may be stopping xtals from forming during the first precipitation with citric.


You could be right but the citric goo is great for decanting (which I think you mentioned). However what is interesting if you look at my last photo of the decanted EA that was left over night, is that now, after 36hours the goo has disappeared and crystals have formed in its place. They still have a little orange attached to them but appear much cleaner. So if you want citrate crystals let it sit for a day and a half and the goo seems to convert and grow crystals. Slow precipitation may facilitate the same thing.

Loveall wrote:

I wonder what would happen if you dissolved your freebase dry harmala candidate in EA, and added citric. Do you get xtals or a goo again? I'll try this when I get a chance.


If i have time I'll try this today with fresh EA.



Loveall wrote:

1) Tried this and only saw floating ice, no FB forming at the bottom 👎
2) I washed a pull with water 3 times. Doesn't work, still got oil when adding citric 👎. However, I reserved a portion of the washed solvent and salted with Fumaric acid. That is giving a yellow/brown precipitate that is xtaline. Will report back on how it looks after decanting.


I wondered if fumaric acid would work, I tried it on my EA after i used the citric acid on it and separated but nothing extra formed. So that is interesting.



Loveall wrote:

3) The fully dried extract with CaCl2 is interesting. A bunch of yellow stuff crashes when the water is removed and can be seen between the white CaCl2 pellets (see image below). Nothing crashes out of the dry solvent when salting with citric (?) but perhaps I was impatient.


Could the CaCl2 have dragged in FB harmala and that's the reason citric acid didn't crash it out???

When I dried the EA for reuse it remained white. (but it had also been washed with sodium carbonate). So that may be irrelevant.

Loveall wrote:

Salting with Fumaric did crash white xtals quicky. Dissolving the organic acid is a lot slower in dry EA. Perhaps harmala citrates like to form with water and that is why they are oily in the raw wet extract and not showing up quickly in the dried extract. Fumaric acid does not seem to have this issue. However, the citrate oil is great for decanting and is perfectly fine since for a quick FB conversion in water.



Water could be playing a role but for the way i did it, water would be in very small amounts. I can test this as mentioned beorfe by dissolving my end product in fresh EA and salting with citric acid. If it doesn't crash out, water is playing a role and i can add a tiny bit and then see if it forms.

I agree warmer pulls are the way to go.
I also agree longer soaks may facilitate for a better extraction.

Loveall wrote:

Finally, the paper in post #2 claims that harmaline can be pulled with EA when basing with sodium bicarbonate. That is surprising, but also interesting. Harmalol my also be pulled under those conditions and could also precipitate when salting 🤞


Haha I have read a few of your posts on harmalol it would be cool if it could be easily pulled and separated. But great stuff Loveall. I think we are off to a good start.
Disclaimer: All my posts are of total fiction.



 
_Trip_
#11 Posted : 9/1/2021 12:36:53 AM

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Loveall,
I dissolved 200mg of harmala in 100ml of EA and added 500mg of citric acid. First FB harmala is way easier to dissolve in EA when warm, I had to give it a bit of time and shake it. It's not as easy to dissolve as I would have thought so longer warmer pulls is definitely the way to go based off this little experiment.
Water is what is causing the goo, without water present it precipitates very nicely into tiny powder like crystals. So like the Cielo tek i would wager less citric acid and longer wait time equals bigger crystals.
Edit: water is likely not what is causing the goo.

However, A little bit of water in the extract isn't a bad thing as it makes the EA decant from the goo very easy. And what doesn't crash out can be left aside overnight. Where as it would seem dry solvent creates crystals that don't seem to want to stick. The harmala citrate in EA acts very much like FB harmala in sodium carbonate saturated water. Having said that the other side of that may mean that the water is dragging in impurities but the end result does look clean and it looks like only harmala crashes out when basing.

To summarize drying the solvent may facilitate a cleaner harmala citrate formation but will require an extra filtering step.

*The citrate appears to hold an off tan colour as well.

Photos will be uploaded later.
Disclaimer: All my posts are of total fiction.



 
Loveall
#12 Posted : 9/1/2021 12:56:22 AM

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_Trip_ wrote:
Loveall,
I dissolved 200mg of harmala in 100ml of EA and added 500mg of citric acid. First FB harmala is way easier to dissolve in EA when warm, I had to give it a bit of time and shake it. It's not as easy to dissolve as I would have thought so longer warmer pulls is definitely the way to go based off this little experiment.
Water is what is causing the goo, without water present it precipitates very nicely into tiny powder like crystals. So like the Cielo tek i would wager less citric acid and longer wait time equals bigger crystals.

However, A little bit of water in the extract isn't a bad thing as it makes the goo decant very easily. And what doesn't crash out can be left aside overnight. Where as it would seem dry solvent creates crystals that don't seem to want to stick. The harmala citrate in EA acts very much like FB harmala in sodium carbonate saturated water. Having said that the other side of that may mean that the water is dragging in impurities but the end result does look clean and it looks like only harmala crashes out when basing.

Photos will be uploaded later.


Cool! I must have been impatient then with my citric acid salting.

I can dissolve what crashes out when drying with CaCl2 in water and pull with EA. Some of the impurities should move into the wet EA layer. I'll salt with citric and see if anything crashes. If no, them I think we can say drying the EA does not help remove impurities from the otherwise orange goo.
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#13 Posted : 9/1/2021 1:03:08 AM

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I found shaking the jar helped it crash out much faster, no surprises there. I think dry EA should give cleaner harmala citrate alternatively one can wait 36hrs and the goo appears to crystalize anyway.

I do like the ease of decanting the sticky goo though. And by the time it is based to precipitate it may not matter whether it is dry, wet or left for 36hours, as the impurities may get stuck in the sodium carbonate saturated water anyway.

The harmala citrate is very fine and although 90% precipitated its still a little cloudy and doesn't want to quite settle. Hopefully not much is lost when filtering.

To add Loveall, the goo maybe a mystery. I added water to my clean EA and harmala citrate no goo seemed to form, maybe its a ratio thing or a saturation thing or it could be due to another alkaloid.

My guess now is that something is causing the harmala to form a goo and it is likely lost when basing with sodium carbonate. But it makes for an easy decant.
Disclaimer: All my posts are of total fiction.



 
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#14 Posted : 9/1/2021 10:19:40 AM

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Quick update:

Here's the citrate that formed when the decanted EA was left for over 24hours:






Here is the end result cleaned up and a comparison with the 200mg FB that was mixed with clean EA and salted out with citric acid.





The cleaner 200mg FB conversion yielded 560mg harmala citrate (I believe at least 20mg was lost during filtering), so at a rough estimate 180mg FB = 560mg citrate.

The harmala citrate recovered from the decanted EA (that was left over night) yielded 240mg (which should be very approximately 60mg of FB). This was cleaned with fresh EA.



Too summarize, from 66g of Syrian Rue seeds

A total of 3.28g of Harmala Freebase was yielded over three runs with the same 66g.
1st cold EA run = 816mg FB
2nd warmer EA run = 1.626g FB [& 240mg citrate (60mg FB approx)]
3rd warm EA run = 780mg

Totals 3.282g of FB Harmala. This equals a total of 4.9% yield.


1st and 2nd run in the vial, 3rd run in the jar.



However, I must note that there is still potential to do another run on the 66g of Rue and there is citrate crashing out of the decant EA from the 3rd run.

What I need to figure out is why the 3rd run came out more impure (based on color anyway) as it appears much more tan than the first 2 runs.
I believe this may be to 4 reasons:
1.Warmer pulls on the third run were too long (5mins, 5mins, 20mins, 5mins 5mins), 2nd run was completed with 4x 2min pulls. Seeds where also compressed more with the french press this may have pushed impurities into the EA.
2.After harmala citrate goo formed it was mixed with water and based (vinegar was not used this time). I doubt this changed anything.
3.A lot less water was mixed with the goo before it was based and shaken. The aim was to see what would happen if it was more concentrated this may have forced more impurities into the FB harmala.
4. Reused EA (was darker) may have not been cleaned enough. However the 2nd run got the lightest colored harmala FB, even over the 1st cold pulls and it had been washed and reused.

Considering this TEK is quite rushed through each step especially when precipitation citrate and FB harmala this can yield good results if one is in a hurry and only one filter step is needed.
Disclaimer: All my posts are of total fiction.



 
Loveall
#15 Posted : 9/1/2021 2:17:48 PM

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3) Makes sense, less water may be the reason the 3rd pull had more off colors. Maybe washing with dilute ammonia will remove the off colors?

So 200 to 180g of FB gives 560g of citrate? That is a lot, I don't understand the stoichiometry. Only thing I can think of that fits is the dihydrogen salt (like we think we have with mescaline), plus 10 water molecules or so (decahydrate) 😮. Will try to reproduce the results.

About the mystery of the red goo. Could be anything of course. Based on your results, the basing step removes whatever makes it gooey, so there is a way to take care of it. I agree the water alone does not cause the red goo.

I am seeing more xtaline results with fumaric, that salting option may be cleaner and require less water rinsing after basing and collecting FB (?).

One reason we may want to avoid the red oil and go for the less colorful xtaline fumaric, is for THH conversion. The cleaner the better, so the zinc only has to work on harmaline without other stuff potentially interfering. If conversion can be done dissolving the EA precipitate in vinegar and stirring with zinc this could be a great shortcut, especially if the end result is pure after basing.

💚🌵💚 Mescaline CIELO TEK 💚🌵💚
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#16 Posted : 9/2/2021 12:38:01 AM

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Yeah I thought 3) was the most likely. More water may facilitate a cleaner product (vinegar may have helped?? but i doubt vinegar did much).

Yeah about 180mg made 560mg very approx (not every crystal was scraped up and a little was lost during filtering) but yeah surprised me. However, I'm not familiar with the chemistry calculations here.

Fumaric acid might be the way to go, but i would imagine it doesn't stick and would need filtering as it couldn't be decant easily.
Definitely worth investigating.

Loveall wrote:
One reason we may want to avoid the red oil and go for the less colorful xtaline fumaric, is for THH conversion. The cleaner the better, so the zinc only has to work on harmaline without other stuff potentially interfering. If conversion can be done dissolving the EA precipitate in vinegar and stirring with zinc this could be a great shortcut, especially if the end result is pure after basing.


I definitely think once we iron out a few more kinks that we could get quite a purer product with the EA and then potentially conversion may become a whole lot easier. This Tek can be done quite quickly as I'm sure you are aware. And as for the precipitation of the EA (with citric acid anyway) one can separate the bulk harmala in under 10mins with only a 3.6% loss compared to leaving the left over EA to sit for 36hrs. Even once based, precipitation of FB harmala can be accelerated by cooling in a freezer just got to work out how to consistently get cleaner looking harmala adding more water to the salted precipitation could help (potential vinegar could be doing something as well).

I think on my next experiment I'll be testing this:
-Fumaric acid
-Citric acid with more water before basing
-Citric acid with vinegar and water before basing
See what comes out cleaner
Also I'll aim to use 1l of fresh EA instead of 500ml, this may bring down the amount of runs to one instead of 3. With warmer pulls.

Also worth investigating is long room temp pulls vs shorter warmer pulls.


I think I'll keep to basing prior to microwaving for now as it seemed to work.


To update the current tek I'll be following for the 2nd attempt will look like this:

-Take Syrian Rue seeds, blend them up into a powder. 100g in total.
-In a separate glass container 300ml of water will be added to 25g of calcium hydroxide (pickling lime) and mixed thoroughly.
-The ground up rue seeds will be added.
-Mix placed in the microwave and put on for short bursts of 3 mins (750 watts) and mixed in-between. Until two thirds of the water content is evaporated.
-Warm water bath for ethyl acetate
-1l of warm EA split into 5 pulls min 2mins each (maybe experiment add a bit more EA and leave the 5th pull in for a longer time).
-Decant ethyl acetate pulls with a french press.
-Combine ethyl acetate and filter.
-Add citric acid (20g per 1l) shaken vigorously.
-Decant Ethyl acetate.
-Add warm water to the citric acid 500ml minimum.
-Slowly base with sodium carbonate and shake.
-Let cool for precipitation.
-Filter and dry


(I will also put 200ml of pulled EA aside and test fumaric acid)
(I will also split the citric acid warm water step into two jars and test one with vinegar added and one without. And see which end result comes out cleaner.)

Disclaimer: All my posts are of total fiction.



 
Loveall
#17 Posted : 9/2/2021 2:26:20 AM

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Looks good. I would suggest dilute ammonia washes at the very end to see if they whiten up the product.

I don't think vinegar does anything, but I could be wrong.

Fumaric seem more xtaline, but the xtals are still reddish (see image below of fumarates precipitated from EA pull). They are also sticky and easy to decant. However, using with citric also seems fine to me.

Here is what I'm doing, a litte different from your pioneering process so we can both learn (differences from your original process in bold):

-Take Syrian Rue seeds (not blending them), 50g.
-Dissolve 15g of sodium carbonate in 150ml of water.
-Add rue to alkaline water
-Microwave for short bursts of 3 mins (750 watts) with mixing until there is no more free running water and the seeds are moist/swollen (about half of the water content is evaporated).
-4x room temp EA split at room temp for 12+ hours each.
-Decant ethyl acetate pulls with a french press and combine (no filter is necessary for whole seeds, but the pulls are longer)
-Add fumaric acid (~5mg per ml) and rest overnight
-Verify ethyl acetate is acidic, decant, wash with a small amount of ethyl acetate, and allow to dry.
-Add warm water to the precipitate until it dissolves completely. Note: if conversion of harmaline to THH is desired used vinegar instead of water and magnetically stir with excess zinc overnight.
-Slowly base with sodium carbonate to pH11.
-Let cool and precipitate
-Catch FB precipitate in filter, wash precipitate in filter a few times with ~2% ammonium hydroxide until color stops changing (stops being wicked away), and dry.

I'll also try grounding the seeds, that may be a lot faster when it comes to pulling, but could be messier. Wanna see how white the product comes out with whole seeds. I've verified whole seeds take time to extract, but it does seem to work as the pH paper in the solvent gets greener as the horus go by.

If the end product is pure, this would be a good practical tek (and grounding the seeds could be much faster if that does cause impurities oh). The simple water extraction + basing to produce crude product would still be faster I think, but this may be as pure as the longer manske/basing TEKs - not sure, depends on the purity we get.
Loveall attached the following image(s):
IMG_20210901_214105942.jpg (677kb) downloaded 384 time(s).
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
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#18 Posted : 9/2/2021 2:57:40 AM

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Loveall wrote:
Looks good. I would suggest dilute ammonia washes at the very end to see if they whiten up the product.


See if I can source any. I did however take the dirty harmala from the 3rd run and dissolve it in a vinegar water mix 500ml total 1:3 and base it out. It's precipitating now and appears much cleaner. Will confirm once filtered but may indicate more water is better when dissolving citrate or fumarate harmala before basing.
However, I haven't been measuring my ph, could this have been the reason for a more impure result?
Edit: The harmala came out much cleaner but still slightly darker than my second run in the photo above.


Loveall wrote:
I don't think vinegar does anything, but I could be wrong.


I would agree but I'm keen to test it side by side just to be sure.

Loveall wrote:
Fumaric seem more xtaline, but the xtals are still reddish (see image below of fumarates precipitated from EA pull). They are also sticky and easy to decant. However, using with citric also seems fine to me.


That's an awesome result, it appears cleaner and as easy to decant definitely a bonus.
(The citrate weirdly becomes cleaner if left to cyrstalize aswell).

I like the look of your process Loveall very keen to see how you go.

Loveall wrote:
If the end product is pure, this would be a good practical tek (and grounding the seeds could be much faster if that does cause impurities oh). The simple water extraction + basing to produce crude product would still be faster I think, but this may be as pure as the longer manske/basing TEKs - not sure, depends on the purity we get.


Well I hope you get a result worth sending off for testing, if deemed appropriate. But IMO I find this much easier and quicker to be honest over the manske teks, so much filtering and rebasing and reacidfying etc. So fingers crossed it delivers a good result. I just looked at the crude tek, that does seem like a fast tek.

I'm not familiar with ammonia washes but it sounds like something i should have been doing.

Disclaimer: All my posts are of total fiction.



 
Loveall
#19 Posted : 9/2/2021 10:14:59 AM

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If you don't have ammonia, I believe a 0.5% Na2CO3 solution is fine to use for washes. Some folks use plain water also, but not sure of that washes away a small amount of harmaline (I just use 2% ammonia, and that is what I have experience with). I don't think the pH will affect purity much, but ideally I like to stop basing at ~ 11.55 (not 11, sorry that may be a little low for harmaline) in the unlikely event that there is a compound that precipitates at higher pH. In general, I try to stop at pH that fully grabs the product (~two units from pKa) and not go much further since you never know if an unwanted protein/compound with a different pKa is waiting to participate beyond the pH that is needed).

I was thinking that another thing to try is completely dry the based rue before pulling with EA. With mescaline, this seems to cause issues (and white xtals can be obtained without the work of drying the cactus paste anyway). However, harmala FB may be OK with drying and going into EA based on your previous result (mescaline "FB" seems temperamental when dried).

I say this because while the CaCl2 solvent dry was somewhat cumbersome after extracting (a lot of water and junk crashing), what precipitates after drying the solvent with fumaric was much cleaner (see image below) compared to the red sticky stuff we get from wet solvent pulls. Note: I tried again to crash the CaCl2 dried extract with citric and that worked only after I added a couple drops of fresh water, but the citric xtals had more of a yellow color compared to fumaric.

So I'll also give this a shot,

-Grind of rue seeds, add ~1/4 parts sodium carbonate, and ~1.6 parts water to form a wet paste, mixing for at least 10 minutes
-Dry paste in microwave
-Optional: add some CaCl2 pellets to the dried paste as "water insurance" during the next step.
-Pull 4-5x with dry EA, warm pulls are faster (warm batter bath)
-Salt with fumaric acid (or citric + a few drops of fresh water)
-Collect precipitate and wash with fresh EA
-Dissolve precipitate in a small amount of warm water. Note: if conversion of harmaline to THH is desired, use vinegar instead of water and magnetically stir with excess zinc overnight.
-Base with sodium carbonate to pH~11.55
-Collect precipitate and wash with 2% ammonia or 0.5% sodium carbonate (squeeze wet filter by folding it into paper towels to wick away traces of sodium carbonate and/or speed up drying)

This product may be pure (or it could have unwanted alkaloids, IDK). If pure, and yields are good (and the THH conversion goes well), it seems like a very nice shortcut (as we have been discussing).

PS: This process is start to look similar to some bufotenine TEKs that use acetone and Fumaric/citric. Harmala FB are not very soluble in acetone, so using EA makes sense.
Loveall attached the following image(s):
IMG_20210902_061847886.jpg (580kb) downloaded 356 time(s).
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
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#20 Posted : 9/2/2021 11:46:58 AM

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Great work Loveall,
that pic is very similar to how the harmala citrate looked when the end product was redissolved in fresh EA and crashed with citric acid. I unfortunately didn't take a photo. But CaCl2 drying looks like it help clean out a lot of gunk. I might have to incorporate it into my next run.

Anyway, I too was wondering what would happen if one was to completely dry out the base mix. Drying it out in the microwave by two thirds seemed to work well for me, drying it out further could stop the EA from getting loaded with water and the gunk that comes attached to the water. So yeah it might be 'purer' end result.

Weird that you had trouble crashing the harmala citrate until you added water. I had no issue when I converted the FB harmala too citrate. Could this have something to do with FB harmala being hydrated or something? (excuse my poor chemistry understanding).

I'm excited to see if THH is easily converted. I don't have a magnetic stirrer or zinc so I can't test this.

I'm not familiar with bufotenine's tek but yeah it is quite similar indeed.


Disclaimer: All my posts are of total fiction.



 
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