Original Manske/Hasenfratz (Fritzsche) Extraction procedure

[Aum_Shanti]

Hi,

Up til now, I only took my Harmalas by a cold tea extraction with some Vit C.

But as I'm now interested in a THH conversion, I wanted to extract.

As I had never any filter clogging problems with my tea, I never understood why you people all moan about it. I thought it's probably because I don't boil my tea.

When I saw, the original Manske extraction, I realized that he also didn't boil them. So I thought give it a try.
He takes ground seeds to acetic water 1:3 (first pull) and 1:2 (second pull).
Up til now, for my tea I rather extracted like 1:30.

So I made this 1:3 stuff testwise with 20g seeds. And I just thought:
"Is this a joke?, That's way not enough water???"

The ground seeds immediately soaked up all the water and formed a semi solid blob, similar to whipped cream. After an hour I could put my beaker upside down and nothing would happen (all stays in the beaker), just like whipped cream would.
Should that really be like that. That seems to me like really way not enough water in this tek???
Is there any disadvantage to going back to my 1:30 ratio. Sure you would need more NaCl for the salting, but that doesn't cost you anything.
OK maybe the losses for the salting would be a bit bigger. But I don't think that much.

As I first did a Manske on my usual tea, and it delivered quite some crystals. But as I was using Vit C for my tea, the Manske crystallization took forever...(several days)

Any thoughts/comments welcome.

Edit:
Hmm, had a look at the original Text from Alkaloids 2, and there he really describes exactly that:

The seeds swell as they absorb the liquid and form a thick dough which is pressed after 2-3 days.

Strange. I really wonder why he did it like that, and not with more water?
What's the advantage for that?

BTW: When people speak about yield of Harmalas e.g. 4-6%. Do they mean FB or HCL weight? What's the difference in weight of these two? Similar to DMT, like about 20%?

 

[Jees]

Can you please refer the tek you speak of, I can't find it in nexus wiki?

My first impression is that you mix "making a tea of seeds" with making "a manske of such a tea." Those are not the same. One never performs a manske on the seeds materials itself. First make tea however you like, cold soaks on powder works, then discard the seeds materials, then on can evaporate to reduce volume, and manske that.
But I do it differently, I do a series of A/B 's until the base liquid is clear (and I filter each acid stage too), only then start doing my many manskes.

Theoretically 100 mg harmineHCL contains 85.3 mg FB.
But you can't avoid salt contamination so in real it might be lesser FB in there.

 

[Aum_Shanti]

Thanks for your reply!

By makling tea I mean that after soaking I filter it, and that's it (a pure yellow liquid, which I then usually drink).

Then I did for testing once a salting (Manske) on it, which yielded these yellow/golden crystals. Why reducing the volume before salting?
I know that some results showed there remains a bit in the salt solution. But AFAIK noone ever tested how much, or did someone?

The original Manske tek isn't in the Wiki. Just in the Alkaloids book (Vol 2, p393):

The crushed seeds of Peganum Harmala are covered with three times their weight of water containing 30 g of acetic acid per liter of water . The seeds swell as they absorb the liquid and form a thick dough which is pressed after 2-3 days. The pressed seeds are once more treated as above with twice their weight of dilute acetic acid and, after maceration, the liquid is again pressed out. To the combined liquors, sodium chloride (100g. / liter of liquid) is added to transform the acetates of harmine and harmaline into the hydrochlorides which are insoluble in cold sodium chloride solutions and are precipitated during cooling. The supernatant liquid is siphoned off, the crystalline residue filtered with suction and redissolved in hot water.

Addition of sodium chloride to the filtered solution causes the precipitation of the hydrochlorides as a crystalline mush and this process is repeated until the hydrochlorides have acquired a yellow color. The final product is then recovered by filtration.

The thing is, that I would actually like to test how much difference there is between boiling and cold extractions, and if the filtering problem is caused by the boiling, or by using acetic acid (instead of Vit C, which I always used for my teas).
But as said I think the original Manske tek is very strange, for it only uses that much water to make a Harmala dough. Don't know what is the idea behind this (as you cannot even stir it), why Manske does it that way.

 

[syberdelic]

I can't speak to the specific tek, but in general terms:

Heating proteins in aqueous solution can cause them to bind to one another and other matter more effectively. This has in the past caused me much filtration headaches with other extractions. A defatting step added under acidic conditions will remove a portion of those proteins.

Aqueous extractions are best done incrementally. A single high volume extraction will always pull more than a single small extraction, but a series of small extractions will beat them both by a large degree. I will usually perform the series of small extractions until I get to the point of diminishing returns.

 

[Aum_Shanti]

but a series of small extractions will beat them both by a large degree

Beat them both in which relation? Final yield?

I would have rather thought to make 2-3 higher volume extractions. As from the cost view it's basically nothing (no special solvent needed).
The question would in this relation really just be: How much of the alkaloids stay in the salt solution? If it is much, then processing small amounts makes big sense. If not, then IMHO processing big amounts makes handling easier.

I'm wondering if this is the reason why Manske did this strange dough tek.

If this is the case, then doing it as Jees, would probably be wiser: First A/B and only later a Manske with little amounts of water.
But the (repeated) Manske first certainly has the advantage to already purify the output a lot, for basically no cost, and no harm potential during handling (as in a A/B).

 

[syberdelic]

I don't know about this case specifically. You very well could be exactly right.
The only reason I try to keep my aqueous volumes reasonably low is because these volumes can add up quickly and become very laborous to work with.

 

[Jees]

... these volumes can add up quickly and become very laborous to work with.

^^^ and that is the reason of evaporating to reduce the volume.
People who do like 3 boils on the seeds, and collect those boils, that is a too large volume so evaporating makes it workable.

One can work with very small volumes if you PRESS that volume out of the seeds, that works wonderful I've noticed.

Pressed boiled liquids are very hard to filter, even absolute vacuum filtering might not work. The only way around it is to let it settle for 12 hours and skim off the top layer. Not poring like decanting as that moves the bottom layer too much.

Don't overthink it too much, you could also follow a nexus wiki tek down to the T.

 

[Jees]

...The original Manske tek isn't in the Wiki. Just in the Alkaloids book (Vol 2, p393)...

Also, it's a good habit here at Nexus to provide a link to your complete source, so anyone can enjoy where you're coming from. :thumb_up:

 

[Aum_Shanti]

Also, it's a good habit here at Nexus to provide a link to your complete source, so anyone can enjoy where you're coming from

I only had this excerpt, which I found once online.
It needed quite some time, but I now found a working public link to the book on the Indian National Agricultural Research System (you just got to love the internet):

The Alkaloids Vol 2:
http://krishikosh.egranth.ac.in/bitstream/1/21370/1/42406.pdf

And if it is of interest:

Vol 1
http://krishikosh.egranth.ac.in/bitstream/1/2023729/1/BPT9916.pdf
Vol 3
http://krishikosh.egranth.ac.in/bitstream/1/21369/1/42405.pdf

The later books aren't available there...

Edit: As i now read the original in detail, the original tek is actually from Hasenfratz.
But this book I couldn't find (Annales de chimie, 151, 1927)

Lol, so it should actually be named to make a Hasenfratz, not a Manske, when salting

Edit2:
So did the first filtration of the "Harmala dough" after 2 days of soaking. Well I had to take a "sock" (yes, really...) to filter, as I couldn't really use anything else to press it out.
Delivered 40ml of heavily contaminated extract (still much particles in it). Don't want to filter again through finer filters as just too much would stay in the filters IMHO.
So I did a Hasenfratz on them (added 4g NaCl), after heating on steam (room humidifier).
Now I also understand why Hasenfratz said to only add 1:2 acetic water for the 2nd pull, as that is exactly what is missing after the pressing. The rest remains in the pressed seed dough.
So it seems I'm more or less as expected with the tek.

As said will later do the same but with a much higher seeds/water ratio and then again with boiling. All on the same seed batch. So results should be comparable.

Edit3:
Ok, after some thoughts...I should have first waited until it settled and the siphoned off, that would have gotten most out without too much loss in filtering. Too late now...

 

[Jees]

Thank you for searching it up :thumb_up:

The krishikosh links don't work for me now, will try again later.
You can upload pdf files in a post also. Worth a try?

 

[dreamer042]

Thank you for searching it up :thumb_up:

The krishikosh links don't work for me now, will try again later.
You can upload pdf files in a post also. Worth a try?

I gotchu. Here ya go. :thumb_up:

 

[Aum_Shanti]

Yeah was the same for me. Seems like the server is rather often down (india...).
But trying it later worked for me.

But it has been posted here now anyways.

BTW: Why I didn't wanted to attach them:

I'm unsure about copyright policies here. So as I don't want to break any rules, I'm rather hesitant to upload such material here.

 

[Jees]

Thank you both :thumb_up:

 

[Aum_Shanti]

Darn it.
Had to throw it away.
It just is sooo difficult to filter it, if you have such a small amount of liquid with such a big amount of seed mush. Fine filtering without discarding most is really extremely difficult.

IMHO this original extraction tek is simply no option. Far too problematic...at least for myself...

If you have more water, you can simply syphon off, but with this tek that's just no option at all.

Will still try my "cold" extraction vs boiled extraction to see the differences.

 

[Jees]

Don't worry, we all had a nightmare on SR and filtering welcome to the club.
Settling and siphoning off rules in such cases.
To make siphoning off easier you can tinker something like this: Jars: seal the lid, make a siphon-off jar.
That .avi shows a powered rue jar with 100% non filter-able top layer settled for 12 hours at least.

 

[Aum_Shanti]

Actually I'm currently doing something similar, only that I use a syringe needle in the front for sucking off to have as less disturbance as possible. But as I saw, you made something similar sometimes.
But I also usually use a little membrane vacuum pump as help.

But with the "dough" tek, this doesn't work, as there is no water on top of the mush...You basically really just have a wet Harmala dough...and to get the little water out clean is a real big problem. At least for me...

So IMHO no problem that it didn't work. I was just curious about this original tek from Hasenfratz. But IMHO it is just unpractical.

 

[Aum_Shanti]

I'm currently going through the Harmala threads (there are really a lot...), and IMHO there are a few things very interesting.

E.g. that it has been discovered that basically cold extraction works just as well as boiling extraction, at least for Caapi. Just the time frame is certainly different. He used 3 days per cold extraction vs 45min per boil.
Cold Acetic Acid Extraction of Caapi

I would actually expect the same result for Rue. But I am at testing...But as said 3 days per soak (which I'm also doing), takes some time.

Another thread is IMHO also interesting. Where someone discovered that actually the boiling is the culprit for getting massive filtering problems. When you just use hot, non boiling water, you don't get the problems.
Cold/Warm Water >>> Boiling water, frustrated filtering

Unfortunately, it seems a test is lacking to see, if the extraction yield is just as good like that. This is a "has to be done" IMHO.

Also interesting is the thread, where someone charred the stuff,where it seems like an extraction could be made easier like that.
Peganum Harmala No Manske Extraction Experiment

Although I'm a bit hesitant about this tek. The temp descriptions are certainly completely wrong (e.g. boil at 230C ???). But maybe some refinement could yield an interesting tek.
E.g. I could think that just after the 1st NaCl salting and FBing it, one could do the charring in an oven, which should get rid of all the substances (oils, etc.) not as stable, and then you could get a purifying tek quite efficient and food grade.

Also this tek for purifying seems very interesting to me. Seems to be quite efficient.
Possible new tek for almost anything

Although some points aren't quite clear to me. E.g. you start with FB, when then adding citric acid, is that right?
Isn't there quite an amount remaining still dissolved in the water part? Or is this similar like the NaCl salting, just with acetone instead?

Also someone posted a google book link to a book from 1847 and I was very surprised to see that all this NaCl salting tek was already in there. So neither Hasenfratz nor Manske were the originators of this tek.
(I added the relevant excerpt of this book to this post)

In it there are IMHO a lot of very interesting points. E.g. that the amount of NaCl needed for salting is dependent on how acidic your solution is. The lower the pH, the more NaCl you have to use. Actually when I think about it, it makes quite sense.
Also that there are also other "things" you can take instead of NaCl for the precipitation step. But NaCl is surely the easiest available and food gradest (does this word even exist?) substance.

 

[Jees]

Thanks for that. Interesting but too much loose ends in those threads. Renders me into sticking to the good ole trusted approach. Only that acetone job on mesc I'll re-read for sure.
:thumb_up:

 

[Aum_Shanti]

I think I will try one or the other tek once, just out of curiosity.

BTW: FBd my 1st cold extraction. Yield was 0.951g FB (surely not yet pure, but already quite bright) of 20g seeds.
Did just one Manske after extraction, and then a FB, then pressed it dry in filter paper (to get as much sodium carbonate out as possible), then 2h oven dried (which made it very fluffy).
Currently the 2nd extraction Manske is running...but I honestly expect a much smaller yield, as the water was way less yellowed than the first.

Lol my first Harmala FB extraction so far. Did always just do a tea before...
BTW is it normal that after FBing the first time, that there still remains some fluorescent yellow in the water? Added an awful lot of lye after filtering the FB out, but it stayed like that.

EDIT:
Wow the 2nd Manske really looks like there will be nothing. Water is yellow, but now even after several hours in the cool, almost nothing precipped out...(used again 15g NaCl/100ml)
I'm wondering if already basically all stuff got out in the first extraction. Yieldwise it could be.

 

[Jees]

Congratulations

Even the smallest trace of harmalas will make that fluorescent impression, don't worry too much about not recuperating those traces.

The second pre-manske liquid is always less colored because the first was full of quinazolines and whatnot that you just kicked out, which is what you want (when making extractions). So don't think in terms of lower yield at all please, but more pure product, and as that happens your needles will form in more and abundant majestic, visually you will think to raise yield.