Syrian Rue Soxhlet Extraction

[ThirdEyeVision]

Anyone ever done it? I've seen a write up a university did using IPA and they tested it afterwards and it still had the goodies (didn't convert to harmala red)

to be safe I was thinking:
pour ground seeds into soxhlet
pull with water and a splash of vinigar for an hour or until solvent is pulling clear.
Procede as normal extraction.

The benifit I see is using less liquid (ie: 1 liter instead of 4) so no reduction needed.
Don't need to mess with 3 boils.
Guaruntees full exhaustion of material.

 

[soulfood]

Sounds like the best way to go if you have the equipment. I'd be interested in seeing any difference in the amount of undesired matter pulled out of the seeds with the absence of heat.

 

[burnt]

SWIM tried it once with acidic water (with acetic acid). It was a pain in the neck but the soxlet was too full for the amount of material in it. If soxlet was bigger or less seeds were used SWIM is sure it would have worked fine. Solvent extraction might have been more easy to work with too instead of water.

 

[ThirdEyeVision]

SWIM tried it once with acidic water (with acetic acid). It was a pain in the neck but the soxlet was too full for the amount of material in it. If soxlet was bigger or less seeds were used SWIM is sure it would have worked fine. Solvent extraction might have been more easy to work with too instead of water.

What size soxhlet was used? My friend will use his 1000ml soxhlet and mix some DE with the rue to aid in solvent flow. I think he'll use water with acetic acid because he's not sure how to remove the toxins without the salting procedure.

Does anyone know if a Methanol or IPA pull will also pull these toxins?

 

[ThirdEyeVision]

And he's off......
1) 200g. of syrian rue was grinder in coffee grinder.
2) 1/2 cup of DE was mixed thoroughly
3) mixture was poured into 1000ml Soxhlet.
4) 1000ml of water brought to 3-4ph with vinegar was poured over mixture and in boiling flask.

Will update.

 

[ThirdEyeVision]

Its cycling fine now.

FYI: Do not attempt this without DE. It was first tried that way and solvent did not cycle. Material had to be removed and mixed with DE and replaced.

 

[69ron]

What kind of DE did you use? There are different kinds, difference sizes, etc.

 

[ThirdEyeVision]

What kind of DE did you use? There are different kinds, difference sizes, etc.

You know, Im not sure. It is used for pool filtering, has no additives. Purchased 15 lbs for 19 bucks at Lowes.

This link takes you to MSDS.

http://www.kem-tek.com/MSDS/343%20MSDS.pdf

Extraction is almost done my friend says. The siphon is pulling yellow, so Id say another 2 hours.

The water must be super saturated at this point because there are loose particles in it. Would you recommend adding water prior to decanting?

 

[ThirdEyeVision]

Here are a couple pics I thought were cool.

 

[Crystalito]

A rather interesting thread, a soxhlet could indeed exaust the plant matter, the downside might be that it might also extract more of the gunk. Well it remains to be seen!

An idea i had in soxhlet applications that might help is this : If one is to use acidified solvent it might be better if the acid is added in the plant matter. For example if one uses acetic acid and water ,i would put the water in the flask below where the solvent goes, pack the soxhlet with the plant matter and on top of it before the cotton add the acetic acid. Then i would run the soxhlet as usual. This way the acid will move through plant matter slowly being diluted as fresh solvent drips on it until it is emptied in the flask. It might help more alkaloids being converted to the salt form and serving as a "first lower pH extraction" on the material while further ones will be at the pH they would be if the acid was added in the flask. I was wondering if this method could be utilised in other ways ,like instead of the acid using a small amount of another solvent on top as a "first run". Anyway, pretty experimental thoughts and propably useless at the grander scheme of things, but you will be the judge of it.

Better let the soxhlet run till the solvent that comes out is clear. I am eager to see what will be the yield of your experiment.

A side thought to all this : Anyone remember the "zinc + Hcl" method proposed for converting harmine/harmaline to THH? I wonder if one could make using a "one pot method" a simultaneous extraction and conversion : use water acidified with HCL in the flask and add zinc, and run this on harmala. Goods will be extracted from harmala with the HCL water and when it reaches the flask the will be converted to THH with the continuous boiling. Stirring might be needed though.

 

[ThirdEyeVision]

A rather interesting thread, a soxhlet could indeed exaust the plant matter, the downside might be that it might also extract more of the gunk. Well it remains to be seen!

An idea i had in soxhlet applications that might help is this : If one is to use acidified solvent it might be better if the acid is added in the plant matter. For example if one uses acetic acid and water ,i would put the water in the flask below where the solvent goes, pack the soxhlet with the plant matter and on top of it before the cotton add the acetic acid. Then i would run the soxhlet as usual. This way the acid will move through plant matter slowly being diluted as fresh solvent drips on it until it is emptied in the flask. It might help more alkaloids being converted to the salt form and serving as a "first lower pH extraction" on the material while further ones will be at the pH they would be if the acid was added in the flask. I was wondering if this method could be utilised in other ways ,like instead of the acid using a small amount of another solvent on top as a "first run". Anyway, pretty experimental thoughts and propably useless at the grander scheme of things, but you will be the judge of it.

Better let the soxhlet run till the solvent that comes out is clear. I am eager to see what will be the yield of your experiment.

A side thought to all this : Anyone remember the "zinc + Hcl" method proposed for converting harmine/harmaline to THH? I wonder if one could make using a "one pot method" a simultaneous extraction and conversion : use water acidified with HCL in the flask and add zinc, and run this on harmala. Goods will be extracted from harmala with the HCL water and when it reaches the flask the will be converted to THH with the continuous boiling. Stirring might be needed though.

It stopes sometime around midnight last night. The siphon tube was still a faint yellow so there was some goodies left to be pulled but for some reason it stoped siphoning so I shut it down to decant over night.

Looking at the flask this morning I can see a white gunk at the bottom. Not sure what it could be unless some DE made it through. He will now filter to see what it is.

Next on his list.
1) throw in pot and do an egg white wash to pull tannins etc.
2) filter again.
3) carbon filter through a 3 foot tube filled with activated carbon.
4) several salt cleanings.
5) final freebasing.

Any suggestions?

Regaring the zinc/HCL pull/conversion. Hotplate is also a stirrer so what you are saying is pull with HCL instead of acetic acid, add zinc to boiling flask and pull should be converted to THH? Has this been verified? My friend has all but the zinc on hand..... Any local source of useable zinc?

 

[distopia]

An idea i had in soxhlet applications that might help is this : If one is to use acidified solvent it might be better if the acid is added in the plant matter.

No need to do this with acetic acid.
Acetic acid evaporate in the aqueous steam current.
It could be useful with Hcl or citric acid, instead.
But acetic should be the acid of choice in this very case.

Better let the soxhlet run till the solvent that comes out is clear. I am eager to see what will be the yield of your experiment.

Me too, please keep us posted.
A good try could be to run the soxhlet with whole seeds and see if the yield is the same.
Avoiding filtering, DE and clogging problems.


BTW, the DE seems the flux calcined type.
It's the most crystallized with the highest porosity, but it's also the most dangerous.
Please use safety mask, at least FFP3, to avoid any risk of silicosis.

1) throw in pot and do an egg white wash to pull tannins etc.
3) carbon filter through a 3 foot tube filled with activated carbon

1) SR does not have tannins... it's not MHRB.
Egg teck is not useful.
3) 3 foot tube filled with activated carbon? I don't know the size of the tube... but seems to much! Too much AC could also keep alks trapped.
It could reduce the yield a lot.


I suggest (someone please correct me in case).
1) collect the aqueous solution from soxhlet.
2) salt with NaCl
3) weight the yield
4) Dissolve in max 100mL water with HCl.
5) Place the beaker on the magnetic hot plate stirrer, place a bar with few GRAINS of AC... and stir at 50C°, max 5 minutes I think.
6) salt again. Should be clear enough.
7) weight the yield
8) Basify.

If 7 = 3... avoid second salting and go straight to basify.

 

[ThirdEyeVision]

An idea i had in soxhlet applications that might help is this : If one is to use acidified solvent it might be better if the acid is added in the plant matter.

No need to do this with acetic acid.
Acetic acid evaporate in the aqueous steam current.
It could be useful with Hcl or citric acid, instead.
But acetic should be the acid of choice in this very case.

Better let the soxhlet run till the solvent that comes out is clear. I am eager to see what will be the yield of your experiment.

Me too, please keep us posted.
A good try could be to run the soxhlet with whole seeds and see if the yield is the same.
Avoiding filtering, DE and clogging problems.


BTW, the DE seems the flux calcined type.
It's the most crystallized with the highest porosity, but it's also the most dangerous.
Please use safety mask, at least FFP3, to avoid any risk of silicosis.

1) throw in pot and do an egg white wash to pull tannins etc.
3) carbon filter through a 3 foot tube filled with activated carbon

1) SR does not have tannins... it's not MHRB.
Egg teck is not useful.
3) 3 foot tube filled with activated carbon? I don't know the size of the tube... but seems to much! Too much AC could also keep alks trapped.
It could reduce the yield a lot.


I suggest (someone please correct me in case).
1) collect the aqueous solution from soxhlet.
2) salt with NaCl
3) weight the yield
4) Dissolve in max 100mL water with HCl.
5) Place the beaker on the magnetic hot plate stirrer, place a bar with few GRAINS of AC... and stir at 50C°, max 5 minutes I think.
6) salt again. Should be clear enough.
7) weight the yield
8) Basify.

If 7 = 3... avoid second salting and go straight to basify.

My friend has always done an egg wash with excellent results. It's a good clarifier regardless of tannins. It's definitely cleaning something out.

Too much AC. Haven't actually got to that point yet, so good catch. Your step 5 would clean it sufficiently with just a few grains? Literally, a few grains?

He'll be completing tonight. Will keep you posted.

 

[distopia]

My friend has always done an egg wash with excellent results. It's a good clarifier regardless of tannins. It's definitely cleaning something out.
Too much AC. Haven't actually got to that point yet, so good catch. Your step 5 would clean it sufficiently with just a few grains? Literally, a few grains?

White egg contains albumine.
Albumine binds negative charge colloids (tannins) in a ratio 1:2 (1 gram of albumine binds 2 grams of tannins).
It's a quite old teck, called "clarification". Romans used it in the wine-making process.
It's useful with MHRB because roots have a lot of tannins (causing nausea)... but since there are no tannins in Syrian seeds, it's pointless
It could be useful if you plan to drink syrian rue tea, it can actually do something (I don't know) but if you perform a manske (NaCl salting) there is no need at all.
If you have any other information please share, there are always new things to learn.

After a manske you actually get short needle crystals, that's are pretty pure by itself.
Dark coloration is actually linked to some heavy colored molecules trapped during crystal formation.
Nothing toxic btw. First manske extraction is good for ingestion.

AC works on molecular weight. Means that heavier mols are trapped first... but if you use too much it starts to traps a lot of things
You have to obtain a discoloration of the water, it will happen quite fast.
Especially with an hot plate stirring.
Remember, 1cm^3 of AC has a inner surface like a football field (nexus quoting).

 

[ThirdEyeVision]

My friend has always done an egg wash with excellent results. It's a good clarifier regardless of tannins. It's definitely cleaning something out.
Too much AC. Haven't actually got to that point yet, so good catch. Your step 5 would clean it sufficiently with just a few grains? Literally, a few grains?

White egg contains albumine.
Albumine binds negative charge colloids (tannins) in a ratio 1:2 (1 gram of albumine binds 2 grams of tannins).
It's a quite old teck, called "clarification". Romans used it in the wine-making process.
It's useful with MHRB because roots have a lot of tannins (causing nausea)... but since there are no tannins in Syrian seeds, it's pointless
It could be useful if you plan to drink syrian rue tea, it can actually do something (I don't know) but if you perform a manske (NaCl salting) there is no need at all.
If you have any other information please share, there are always new things to learn.

After a manske you actually get short needle crystals, that's are pretty pure by itself.
Dark coloration is actually linked to some heavy colored molecules trapped during crystal formation.
Nothing toxic btw. First manske extraction is good for ingestion.

AC works on molecular weight. Means that heavier mols are trapped first... but if you use too much it starts to traps a lot of things
You have to obtain a discoloration of the water, it will happen quite fast.
Especially with an hot plate stirring.
Remember, 1cm^3 of AC has a inner surface like a football field (nexus quoting).

Great info, thanks.

The egg wash is something he has always done on MHRB and Syrian rue. Didn't know the science behind it, just knew it went in clear came out chunky and brown so figured it did something. I do know 100% it did come out clearer after the egg wash. Now you just got me worried it's clearing out the wrong stuff...

The tube of AC was an idea he had and was going to test it. Scraped. But like the new idea much better. So in 1000 ml is there a formula to calculate how much to use? Or is a few pieces really enough?

 

[ThirdEyeVision]

Acording to wikipedia egg whites remove polymerized tannins, coloring phenols and proteins. I can verify that prior to the egg wash it is not see through but after the egg wash it is clear from experiance.

 

[distopia]

Now you just got me worried it's clearing out the wrong stuff...

I actually don't know what an egg teck could do on syrian rue tea.
It could be neutral... I really don't know.
I know you can avoid it in this very case

So in 1000 ml is there a formula to calculate how much to use? Or is a few pieces really enough?

1000 mL? Quite a lot...
I suggest a Manske teck (NaCl salting) on the crude tea.
Collect the precipitate.
On 200gr seed at 3.5% average you will have maybe 7gr crude extract.
Dissolve this 7 gr in to acidified water.
Less the better! 100mL maybe.

A bag with 100Gr AC can filter several times a 120Liter fish tank...
I think that half coffee spoon on 100mL will be more than enough.
You can also pack a small clarification column.

 

[ThirdEyeVision]

Manske is used.
The soxhlet is 1000ml (reasoning for 1000ml of liquid)
He was going to do the AC cleaning prior to Manske. Guess it would be better to do it after the manske for a reduced amount of liquid.
Egg wash could be pointless but he has been doing it for years and is stuck in his ways I'm telling you though, there is a noticable difference. Have you done it? Your so dead set against it. Try it and see it is cleaning out gunk. From my research it is shown to remove more than just tannins. Even the great Wiki says it cleans more. But no worries, to each his own.

 

[distopia]

Manske is used.
The soxhlet is 1000ml (reasoning for 1000ml of liquid)
He was going to do the AC cleaning prior to Manske. Guess it would be better to do it after the manske for a reduced amount of liquid.
Egg wash could be pointless but he has been doing it for years and is stuck in his ways I'm telling you though, there is a noticable difference. Have you done it? Your so dead set against it. Try it and see it is cleaning out gunk. From my research it is shown to remove more than just tannins. Even the great Wiki says it cleans more. But no worries, to each his own.

Thank you for your posts,
Namasté

 

[ThirdEyeVision]

Did an egg wash with 4 egg whites.
Re-Filtered.
Poured into beaker and brought to boil while stirring (boiled over and lost about 100ml )
poured in salt until no more would disolve: +/- 250g.
Set aside to cool slowly and decant crystals.

Right now it is raining white crystals on top of the initial brown precip. Will let decant over night.