Question about syrian rue extraction

[igorcarajo]

So I'm trying to do a syrian rue extraction following "the tao of rue extraction" and "harmalas extraction and separation guide". I made the tea, then I added NaOH a bit at a time until the whole thing turned milky. Then I let that rest for like a day and there was stuff at the bottom and brown water on top. I poured that over a coffee filter and kept the liquid in a jar just in case. Now the gunk trapped in the coffee filter I put in another jar and then poured a hot 3:1 water/vinegar mix in it. After several hours, it looks like the picture attached. Light colored gunk at the bottom, and pretty translucent brown/reddish water on top. So I want to make sure I understand this right, the harmalas (along with some other unwanted alkaloids) are now dissolved in the water, and the gunk at the bottom is plant matter and whatnot, so I should filter this, keep the water and discard the gunk? Thanks in advance.

 

[Asher7]

The gunk that settles out when you base it is your harmalas, so as I understand you took those solids and redissolved in vinegar and water? If that is the case there should be no gunk or particulates until you do a manske or rebase, whatever you want to do but fb harmalas should totally dissolve in the water and vinegar.

The pic looks like how the alks settle when based, it doesnt look like dissolved harmalas in acidic water.

The only other thing I can think of is how well did you filter it. If that is seed material then you want to get that out but that’s a whole lot of seed material. It looks like based out harmalas.

 

[pastanostra]

I saw on a topic this helping sentence :

" In acidic discard solid, in basic discard liquid "

If you're confident with your acidic is acidic enough, you can pour off solid (keep them in case of..).

I messed an extraction mostly with the same symptoms.
I did not let enough time to reduced teas to settle, then based, discarded solid, dissolved in acidic, and i had a sort of precipitate like in your picture.
Added more and more vinegar and these not dissolved. I resulted with a too much acidic solution that took too much time and effort to come back to a normal way.

For me you tea seems clear and good to be kept. The bottom seems a sludgy powder of rue, did you powdered your seeds ?

Sludge after dissolving in acidic:

 

[igorcarajo]

Thanks for the replies. Well, I filtered out the gunk at the bottom. I guess when I do the salting I’ll find out if the liquid still had harmalas in it or I threw them away.

 

[igorcarajo]

Also I need some clarification on this: in the “Harmalas extraction and separation guide”, step 14 says:

I recommend repeating the steps 10-13 at least 3 times. I also recommend always doing in this alternating order, precipitating the salt, then redissolving in warm water, precipitating the base, redissolving in warm acidic water, repeat again, until its clean enough for you.

So precipitating the salt is the manske? Then you discard the liquid and keep the crystals, then dissolve the crystals in warm water, add a base, keep the solids and discard the liquid, then add acidic water, keep the liquid and discard the solids, then salt it again, and so forth and so on? Am I getting it right?

 

[Asher7]

The cycle from filtered tea is, basify to make solid freebase crystals and filter out the water. Redissolve in vinegar and water and then, manske so crystals form and filter the water. That is so you filter all other material that are soluble in one ph range but not the other.

The time for getting plant solids out is right after you boil the tea or right after dissolving the fb in acidic solution but before the manske while the crystals are dissolved and can get through the filter, but the solid plant matter can’t. (In that instance you keep the water and toss the solids because your crystals are dissolved) Do that cycle 4-5 times, base, filter, manske, filter, base, filter, manske filter etc. You will eventually get white harmala extract with just the slightest amount of tan in it when in fb form.

Also, while I’m thinking about it my additional advice would be to let it sit for 24 hours each time you do a conversion. Freebase takes forever to settle so if you pull it out, in the morning you’ll see additional alkaloids that settled if you don’t toss the water immediately. For the manske let it sit and grow for at least 12 hours and then seal the jar and put it in the fridge for another 12 or so hours. The longer the better I would think as long as it doesn’t spoil from sitting around for 2 weeks at room temp.

One last thing is, I think you lose a portion of product for each manske you do, I’m not sure, but there may be more conservative was of converting the freebase over to a salt using another chemical or method. Most kitchens have salt though so that’s what was used.

 

[igorcarajo]

Thanks. One other question, when you salt it, initially the water is hot and you dissolve salt in it, then you let it cool and eventually you put it in th fridge, and the harmalas will precipitate. The question is, wouldn’t some salt also precipitate along with the harmalas?

 

[downwardsfromzero]

One last thing is, I think you lose a portion of product for each manske you do, I’m not sure, but there may be more conservative was of converting the freebase over to a salt using another chemical or method. Most kitchens have salt though so that’s what was used.

It's likely that a small portion of the harmalas will remain dissolved after performing the Manske precipitation. These could in principle be recovered by adding base, although given the volume of liquid involved versus the small amount of alkaloid it might not be worth the effort.

wouldn’t some salt also precipitate along with the harmalas?

Typically a 20% w/v salt solution is used for the the Manske, which isn't so near the saturation level for sodium chloride, especially after adding to a further volume of liquid. The change in solubility of sodium chloride between hot and cold water is only slight.

A small amount of salt does get trapped in the crystals as they form but most salt contamination will result from remnants of the solution trapped between the crystals after filtration. This could in principle be minimised by letting the solution cool as slowly as possibly, leading to the formation of larger crystals with a relatively smaller surface area.


Has anyone tried recrystallising harmala HCl from water or dilute HCl? This would also reduce salt contamination.

 

[igorcarajo]

One other question: for the finished product, what is the difference between collecting the crystals from the manske, and collecting and drying the precipitate after basifying the liquid? Is one form a salt and the other a freebase? Both the tao of rue extraction and the harmalas extraction and separation guide show the last step to be to basify and collect and dry the precipitate. I don’t understand why you finish with that instead of collecting the crystals from the manske. Thanks.

 

[Asher7]

Yes, after the base step your crystals are freebase and after the manske they’re in salt form. The consensus is freebase is better for smoking while the salt form is better for eating, plugging I believe and a few other roa’s. Freebase is thought to be less stable so therefore not as good for long term storage even though a good number of people have told me that fb lasts a long time if stored correctly so I’m not sure what a reasonable time period would be for expiration.

 

[igorcarajo]

Thanks, Asher7. So if I want to ingest the Harmalas orally dissolved in some orange juice or Coke, I can just keep them in salt form?