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A new level of harmala purity with this extraction
- Thread starter whiterasta
- Start date
soxy bastard
Rising Star
SnozzleBerry said:
Paper chromatography under UV-A with rue shows two major bands and one minor trace band
Similar using Caapi yeilds three main bands and no trace band.
ethanol water extract yeilds up to seven flourescent bands and several visible light markers for rue
similar for caapi yeilds four to six flourescent bands and several obvious tannin markers.
No other analysis has been performed in the wake of the chromatographic match for harmine and harmaline standards for both rue and caapi, however in the abscence of a THH standard it is only assumed the third band found in caapi extract is THH
I am satisfied this method is selective as the manske route within the parameters of crude analysis performed along with selective precipitation from rue F/B yield only harmine and harmaline with the leftover solution nearly devoid of any alkaloids.
Research on whiterasta indicates a past professional carreer in chemistry. And in reading much of his work from the shroomery to the nook he posts in scratch pad lab note form expecting any who read to automatically be up to speed on where ever his mind has wandered.That said in each case he has put forth a tek it has proven itself from introducing KOH in reducing emulsions,this F/b precipitation to what he has shared with chinacat @ the shroomery on the 70's acid scene has been spot on.
I expect he considered the removal of unwanted alkaloids by way of acidifying the menstrum followed by rapid raising the PH having a similar effect as the acidic extraction and halide substitution.
SB
I know this is an old thread but I feel compelled to jump in and say that after doing a Manske NaCl precipitation on an acidified aqueous harmala extract, once the precipitated harmine/harmaline have been removed by decanting/filtering, the remaining solution can be basified (and yes, sodium carbonate is my favorite for this, just watch out for the volcano), and more alkaloids will crash out. They are darker in color and are not harmine and harmaline, they are all the other alkaloids - or degredation products thereof - that are present in harmala.
Presumably the makeup of these alkaloids varies due to genetics, growing conditions, time of harvest, etc.
Point is, there's other stuff in rue besides harmine/harmaline, and the manske NaCl precip separates these. I don't know about whiterasta's tek cuz it uses alcohol, and he never really clarified that part about preciping harmaline salts at pH 6 but it sounds to me like there's at least a possibility that this could extract those other alkaloids.
The way to find out for sure would be to do a whiterasta tek, then redissolve in acidic aqueous solution, do a Manske NaCl precip, remove harmine/harmaline crystals, then basify with sodium carbonate (or lye, ammonia, or whatever, though ammonia fumes are harmful and lye is dangerous so why not sue sodium carbonate when all you gotta do is bake baking soda?). If anything else crashes out, then we know this tek does not isolate pure harmine/harmaline.
I agree, whiterasta's a knowledgeable dude, but we all tend to overlook things sometimes. And he never did really clarify the tek (not pointing fingers here, I've promised to post many things that I still haven't gotten around to... just saying).
Love,
SyZ
Presumably the makeup of these alkaloids varies due to genetics, growing conditions, time of harvest, etc.
Point is, there's other stuff in rue besides harmine/harmaline, and the manske NaCl precip separates these. I don't know about whiterasta's tek cuz it uses alcohol, and he never really clarified that part about preciping harmaline salts at pH 6 but it sounds to me like there's at least a possibility that this could extract those other alkaloids.
The way to find out for sure would be to do a whiterasta tek, then redissolve in acidic aqueous solution, do a Manske NaCl precip, remove harmine/harmaline crystals, then basify with sodium carbonate (or lye, ammonia, or whatever, though ammonia fumes are harmful and lye is dangerous so why not sue sodium carbonate when all you gotta do is bake baking soda?). If anything else crashes out, then we know this tek does not isolate pure harmine/harmaline.
I agree, whiterasta's a knowledgeable dude, but we all tend to overlook things sometimes. And he never did really clarify the tek (not pointing fingers here, I've promised to post many things that I still haven't gotten around to... just saying).
Love,
SyZ
DreaMTripper
Rising Star
DreaMTripper said:
Oh past self did you not read anything?!
:roll:
Am I right in saying these alkaloids are so delicate even acetone oxidises them?
Also, when the freebase is dry will sodium carbonate be a contamination?
No, harmalas are far from delicate - it is that there is not a good, readily available solvent to pull them. DCM works but is not excellent. Naphtha, limonene, xylene etc all dissolve freebase harmalas very poorly.DreaMTripper said:
Precipitating them out of basic solution is really a superior approach to isolate harmalas.
Kerberos
Michael
Hi, did this Tek ever make it to the Wiki if so what is it under?
I am receiving a couple of Kilos from Iran of Syrian rue and would like to try an extraction tek.
I was looking at the Wiki and thought to try the TAO tek. That was until this thread was thrown up with a couple of recent posts.
Was it ever confirmed if this was a better/different final product using this method?
Thank you
Kerberos
I am receiving a couple of Kilos from Iran of Syrian rue and would like to try an extraction tek.
I was looking at the Wiki and thought to try the TAO tek. That was until this thread was thrown up with a couple of recent posts.
Was it ever confirmed if this was a better/different final product using this method?
Thank you
Kerberos
DreaMTripper
Rising Star
Cheers, so just a basic salt saturated solution put in the fridge to precipitate?Infundibulum said:
What pH? Is 11 ok?
No, either you precipitate the base by raising the pH (11 or so is fine yeah), or you precipitate harmala in HCl form by adding salt to an acidified solution.
For quantities and more specific info, check the harmala extraction and separation guide or some other harmala xtraction tek in the wiki.
For quantities and more specific info, check the harmala extraction and separation guide or some other harmala xtraction tek in the wiki.
DreaMTripper
Rising Star
Ok thanks.
Chan
Another Leaf on the Vine
Thought I’d post my attempt at Whiterasta’s tek, as the original is a bit light on details…
In summary, I performed this just after doing a standard Manske, with the aim of comparing yields. I did this tek in slow-time, leaving days between steps, because I had other stuff to do too ;-)
1. Powdered 100g Syrian rue seeds, and mixed with 200 ml Ethanol (95%) with ~0.5 tsp citric acid. Capped jar and let stand for 4 days. Reddish-brown liquid with turquoise sheen in daylight.
2. Strained using an AeroPress with metal disk, and washed solids with 40% ethanol (vodka) to bring total volume of liquid to 330 ml.
3. Ran this thru paper filter twice, which stained very red. Liquid lighter in colour but would probably need 20 attempts to clean completely…didn’t bother with further attempts.
4. Simmered for a few minutes, watching carefully, until alcohol smell disappeared completely. Volume now ~80ml. Added 150ml distilled water to loosen up.
5. Filtered this 5x through cotton wool (also in AeroPress) but still wasn’t crystal clear.
6. Chilled overnight to see if any sediment fell out, but it didn’t.
7. Based with ~25ml janitorial ammonia, to give pH 11. Instant precipitation. Here I tried an experiment: I poured this into a sep funnel I have, and stood it up in the fridge, and left it for about a week. I wanted to see if I could run off the sediment from beneath the liquid: it sorta worked, but the liquid just formed a kind of bore-hole through the sediment, so I got a first rush of sediment, followed by clear liquid, as the rest stayed caked inside the funnel. So, transferred everything to beaker, and let settle again.
8. Another attempt to catch the sediment: placed beaker in freezer on top of pre-cooled metal block for ~30 mins. This worked better, and the bottom of the beaker was frozen solid, so I could pour off liquid and ice-crystals from the top, before adding fresh water, to wash. Washed/froze 3x.
9. After the final washing, I didn’t add any extra water, just ~0.25 tsp citric acid to the wet harmala mix (~50ml) to redissolve harmalas as bright red citrate. Chilled overnight and a little black sediment fell out, which was discarded.
10. Mixed with 0.5 tsp CaOH. Nothing much happened, until I started to heat in water-bath, when precipitates started to form. Heated to about 60C, and pH showed 6-7.
11. Chilled overnight, and re-checked pH, which was now 8, oops! Added a pinch of citric to get pH back to 6-7, before filtering. Quite a bit of tan-coloured sediment. Filtered solution now a clear, bright red.
12. Dried in low oven (85C) for about an hour, yielding 1.3g rust-coloured harmalas citrate. With the earlier Manske extraction, I got about 3.3g freebase, but that was not perfectly pale, so probably not 100% pure.
Conclusion: I think I’ll persevere with Whiterasta’s tek. It’s a lot less messy, and you don’t have big volumes of water and sludge to deal with, which means I should be able to start with a larger amount of seeds. More finesse needed for steps 8 thru 11.
In summary, I performed this just after doing a standard Manske, with the aim of comparing yields. I did this tek in slow-time, leaving days between steps, because I had other stuff to do too ;-)
1. Powdered 100g Syrian rue seeds, and mixed with 200 ml Ethanol (95%) with ~0.5 tsp citric acid. Capped jar and let stand for 4 days. Reddish-brown liquid with turquoise sheen in daylight.
2. Strained using an AeroPress with metal disk, and washed solids with 40% ethanol (vodka) to bring total volume of liquid to 330 ml.
3. Ran this thru paper filter twice, which stained very red. Liquid lighter in colour but would probably need 20 attempts to clean completely…didn’t bother with further attempts.
4. Simmered for a few minutes, watching carefully, until alcohol smell disappeared completely. Volume now ~80ml. Added 150ml distilled water to loosen up.
5. Filtered this 5x through cotton wool (also in AeroPress) but still wasn’t crystal clear.
6. Chilled overnight to see if any sediment fell out, but it didn’t.
7. Based with ~25ml janitorial ammonia, to give pH 11. Instant precipitation. Here I tried an experiment: I poured this into a sep funnel I have, and stood it up in the fridge, and left it for about a week. I wanted to see if I could run off the sediment from beneath the liquid: it sorta worked, but the liquid just formed a kind of bore-hole through the sediment, so I got a first rush of sediment, followed by clear liquid, as the rest stayed caked inside the funnel. So, transferred everything to beaker, and let settle again.
8. Another attempt to catch the sediment: placed beaker in freezer on top of pre-cooled metal block for ~30 mins. This worked better, and the bottom of the beaker was frozen solid, so I could pour off liquid and ice-crystals from the top, before adding fresh water, to wash. Washed/froze 3x.
9. After the final washing, I didn’t add any extra water, just ~0.25 tsp citric acid to the wet harmala mix (~50ml) to redissolve harmalas as bright red citrate. Chilled overnight and a little black sediment fell out, which was discarded.
10. Mixed with 0.5 tsp CaOH. Nothing much happened, until I started to heat in water-bath, when precipitates started to form. Heated to about 60C, and pH showed 6-7.
11. Chilled overnight, and re-checked pH, which was now 8, oops! Added a pinch of citric to get pH back to 6-7, before filtering. Quite a bit of tan-coloured sediment. Filtered solution now a clear, bright red.
12. Dried in low oven (85C) for about an hour, yielding 1.3g rust-coloured harmalas citrate. With the earlier Manske extraction, I got about 3.3g freebase, but that was not perfectly pale, so probably not 100% pure.
Conclusion: I think I’ll persevere with Whiterasta’s tek. It’s a lot less messy, and you don’t have big volumes of water and sludge to deal with, which means I should be able to start with a larger amount of seeds. More finesse needed for steps 8 thru 11.