Why is this necessaray?
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Harmala extraction - unneccessary steps?
- Thread starter Brennendes Wasser
- Start date
Because harmalas are naturally in freebase form inside the seeds, so they aren't water soluble and therefore hard to extract. The seeds aren't acidic and won't make the water acidic, so you need to add some acid to allow the harmalas to turn into salt form and become water soluble.
I think they are in a salt form called tannate, which is obviously why they can be dissolved in water when you make rue seed tea. At this point, I don't know why this first step is necessary when we can boil right away, and it works great.
Are they? As far as I know, rue has no tannins, so it would be surprising if they are in that form (not saying that they aren't in a different type of salt). You may be thinking of Mimosa. And when making rue tea it's usually recommended to do it in acidic water as well (most tap water is slightly basic). But I may be wrong, maybe some more knowledgeable member can help. If it works with no acid, it works, but it would be interesting to compare yields.
As we know from pH separation experiments, harmine can precipitates (means it is in freebase form) in surprisingly low pH, it does not be to be very alkaline, pH 7 is enough sometimes, iirc. So it could be that solubility is lower in neutral water.
Most plants and their decoctions are slightly acidic, so we should be safe, but it is better to keep rue tea below pH 5 by adding acid.
Most plants and their decoctions are slightly acidic, so we should be safe, but it is better to keep rue tea below pH 5 by adding acid.
It may not be necessary but it makes the boils more efficient.
I think they are in salt form bcz rue tea is fluorescent and as far as i know the freebase is not.
Good to know, thanks! And also, for the record, I was just looking up some papers to see if they mentioned anything about the alkaloids being in salt or freebase form, and I found that rue seeds do contain tannins. So I was also wrong on that one.
Andromedius
Rising Star
Thanks a lot for the explanation!
This is my first time doing an extraction, I have a few questions.
So, I boiled 200 g of seeds in a vinegar water solution three times for 30 minutes at 80°C.
Question 1. Is there any point in doing a fourth boil?
I strained the solution through a filtering cloth, because when I first tried using a sieve, I realized the seeds contained some sand.
Question 2. Is the sediment caught in the cloth just waste, or does it have any value?
I'm now at step 3.
Question 3. How long should I wait for everything to settle before decanting the water?
Will what I obtain be freebase? Can I convert it to a salt, and is there any benefit in doing so? And is the result considered full spectrum?
This is my first time doing an extraction, I have a few questions.
So, I boiled 200 g of seeds in a vinegar water solution three times for 30 minutes at 80°C.
Question 1. Is there any point in doing a fourth boil?
I strained the solution through a filtering cloth, because when I first tried using a sieve, I realized the seeds contained some sand.
Question 2. Is the sediment caught in the cloth just waste, or does it have any value?
I'm now at step 3.
Question 3. How long should I wait for everything to settle before decanting the water?
Will what I obtain be freebase? Can I convert it to a salt, and is there any benefit in doing so? And is the result considered full spectrum?
I'm guessing you mean the step 3 highlighted below with arrows?
There might be, if the third boil was still fluorescent enough to completely block the penetration of a UV light beam. UV penetration distance is an easy way of estimating harmala concentration. Concentrated solutions completely block the passage of a beam of light from a UV or deep violet LED because there are enough molecules in the surface layer to absorb all the relevant photons. View from the side to understand this. A more dilute solution will have a noticeable beam penetration distance. Research the term "molar extinction coefficient" to find out more.
So, if your third cook was still sufficiently concentrated to block the beam within, say, 1cm at the most, it's going to be worth boiling the seeds again.
Deep violet LEDs can be obtained easily as kids' "spy pen" toys for reading "secret messages" written in fluorescent "invisible" ink. Powerful blue LED torches are also provided with photoactivated adhesive kits and also do the trick while being considerably more robustly built than the kids' toys. I'd go as far as to say, one or other item like this is almost indispensable
Not just protein, but in this case we can juggle the figures around and (eventually*) come up with both ε for harmala solution and a way of estimating the actual approximate concentration.
[*Detailed technical commentary omitted for brevity. Rue brew is a crude extract and will probably misbehave, as well as having a mixture of fluorescent compounds with differing responses. Even so, harmaline fluorescence generally greatly predominates.]
[I used this method for monitoring pulls on 1kg rue seeds and there was still abundant fluorescence on the eighth PC cook, but my volumes were low because the pan was honestly a bit too small. Don't bother with a cook that big unless you have a lot of container volume with which to work on it.]
It's essentially junk, but you can chuck it back into the boiling pot if you think it might be seed coat with a useful amount of harmalas in it. Test a sample by dropping it into distilled water and immediately observing the extent to which fluorescent material diffuses out, with the help of the handy torchlet you now have (right?)
Test for turbidity with a red laser pointer. If the particulates have settled out, the laser beam will not be visible side-on. Settling can easily take a couple of days in the fridge if you want to be particularly obsessive about it. The alternatives to waiting are simply accepting a less-pure product, or putting your product through another entire A/B cycle - which is more effort, takes just as long, and most likely causes losses. Or use a centrifuge, if you happen to have one.
If you mean settling of the washes on the freebase (step 7) , that goes more quickly.
Step 5 - "adjust to pH 10+" means that the harmala alkaloids will precipit;te as the freebase. "Basic" here means the pH is above 7.
Yes you can, and it will mean you have a water-soluble product that may be more stable in the long term. For some applications the freebase form of harmalas is more desirable.
In absence of any explicit separation step, the product from this "brew, base and rinse" process is going to be 'full spectrum' freebase - mostly harmaline ['DHH'] and harmine ['H'], and usually somewhere between 3:1 and 1:1 DHH:H, with a bit of THH if you're very lucky.
If I'm being honest, I'd suggest it might be better to understand the answers to those types of questions before embarking on an extraction - but you'll be fine pausing at this point with your acidic brew settling happily in the fridge for a few days. That'll help you take care of any further reading you may happen to need to do - in which case, you've got yourself ahead a little bit already so a small pat on the back is in order if you can tell us what you're planning to use for adjusting the pH upwards
Welcome to the Nexus, feel free to introduce yourself!
Andromedius
Rising Star
Wow! Thank you for such a quick and thorough reply. I admit that asking whether it was a base or a salt was a dumb questionI'm guessing you mean the step 3 highlighted below with arrows?
There might be, if the third boil was still fluorescent enough to completely block the penetration of a UV light beam. UV penetration distance is an easy way of estimating harmala concentration. Concentrated solutions completely block the passage of a beam of light from a UV or deep violet LED because there are enough molecules in the surface layer to absorb all the relevant photons. View from the side to understand this. A more dilute solution will have a noticeable beam penetration distance. Research the term "molar extinction coefficient" to find out more.
So, if your third cook was still sufficiently concentrated to block the beam within, say, 1cm at the most, it's going to be worth boiling the seeds again.
Deep violet LEDs can be obtained easily as kids' "spy pen" toys for reading "secret messages" written in fluorescent "invisible" ink. Powerful blue LED torches are also provided with photoactivated adhesive kits and also do the trick while being considerably more robustly built than the kids' toys. I'd go as far as to say, one or other item like this is almost indispensable
Not just protein, but in this case we can juggle the figures around and (eventually*) come up with both ε for harmala solution and a way of estimating the actual approximate concentration.
[*Detailed technical commentary omitted for brevity. Rue brew is a crude extract and will probably misbehave, as well as having a mixture of fluorescent compounds with differing responses. Even so, harmaline fluorescence generally greatly predominates.]
[I used this method for monitoring pulls on 1kg rue seeds and there was still abundant fluorescence on the eighth PC cook, but my volumes were low because the pan was honestly a bit too small. Don't bother with a cook that big unless you have a lot of container volume with which to work on it.]
It's essentially junk, but you can chuck it back into the boiling pot if you think it might be seed coat with a useful amount of harmalas in it. Test a sample by dropping it into distilled water and immediately observing the extent to which fluorescent material diffuses out, with the help of the handy torchlet you now have (right?)
Test for turbidity with a red laser pointer. If the particulates have settled out, the laser beam will not be visible side-on. Settling can easily take a couple of days in the fridge if you want to be particularly obsessive about it. The alternatives to waiting are simply accepting a less-pure product, or putting your product through another entire A/B cycle - which is more effort, takes just as long, and most likely causes losses. Or use a centrifuge, if you happen to have one.
If you mean settling of the washes on the freebase (step 7) , that goes more quickly.
Step 5 - "adjust to pH 10+" means that the harmala alkaloids will precipit;te as the freebase. "Basic" here means the pH is above 7.
Yes you can, and it will mean you have a water-soluble product that may be more stable in the long term. For some applications the freebase form of harmalas is more desirable.
In absence of any explicit separation step, the product from this "brew, base and rinse" process is going to be 'full spectrum' freebase - mostly harmaline ['DHH'] and harmine ['H'], and usually somewhere between 3:1 and 1:1 DHH:H, with a bit of THH if you're very lucky.
If I'm being honest, I'd suggest it might be better to understand the answers to those types of questions before embarking on an extraction - but you'll be fine pausing at this point with your acidic brew settling happily in the fridge for a few days. That'll help you take care of any further reading you may happen to need to do - in which case, you've got yourself ahead a little bit already so a small pat on the back is in order if you can tell us what you're planning to use for adjusting the pH upwards
Welcome to the Nexus, feel free to introduce yourself!
So, the extraction is done. I raised the pH to 10 using a sodium hydroxide solution. I have to say, the process is beautifully magical! Once everything that was supposed to precipitate had precipitated, I decanted until the pH was neutral. To speed things up, I strained the contents through coffee filters and put them in a food dehydrator.
