Travel log: rue extraction (IPA & Phosphoric acid)

[The Traveler]

About a month ago I talked with Phlux- about rue extraction and he told me he used IPA. Curious about that I began experimenting with it together with the use of phosphoric acid. Many things about the use of the IPA are Phlux-'s ideas, not mine.

This thread is my travel log about what I encountered along the way and what I thought was interesting. This is not a written down step by step extraction tek though if you read it well you can use it to extract your own rue.

I tried to log everything with pictures so I hope you all enjoy the ride.



Along the way the posts in this thread might be updated, when that happens I will make a remark about it in this starting post.

 

[The Traveler]

First we pulverize the seeds. I do this in a nice 700Watt blender:

Amount: 50g of whole rue seeds

The seeds in the blender, still whole

The blender at work

And the blended seeds are now a nice fluffy powder

 

[The Traveler]

We now add the IPA.

Amount: 200ml of IPA

The IPA added to the freshly blended seeds

Just after blending them nicely together

After settling a while

And completely settled

 

[The Traveler]

Adding phosphoric acid to the rue+IPA mixture

Amount: 3 drops of phosphoric acid

Yellow clouds forms where the phosphoric acid dropped down

Nice yellow clouds

After blending and settling down again, this is what it looks like

 

[The Traveler]

Pulling the IPA

Slowly decant the IPA from the mixture

The IPA runs through the coffee filter rather fast, there are oils but they don't completely clog up the filter!

SPECIAL NOTE: The oils extracted with the IPA don't completely clog up the filter!

 

[The Traveler]

Drying the IPA

Note: The IPA is evaporated at 70C

The pulled IPA that was filtered

The IPA is poured into a Pyrex dish

The Pyrex dish with the IPA in it in the food dehydrator

The food dehydrator is set at 70C and will run until the IPA is completely evaporated

 

[The Traveler]

Adding IPA + phosphoric acid to the mixture for the second time

Amounts: IPA 200ml + 3 drops of phosphoric acid

The IPA is added...

...and the phosphoric acid is added

Phosphoric acids clouding yellow again...

...but disappearing faster as the first time!

SPECIAL NOTE: This time the phosphoric acid yellow cloud was less and disappeared faster!

 

[The Traveler]

Adding the second IPA pull to the evaporation dish

The IPA from the first pull completely evaporated

The IPA from the second pull is added...

...and getting ready for full evaporation

 

[The Traveler]

Redissolving the evaporation remains in water

Amount: Water 150ml

All IPA is evaporated, a yellow/brownish/fluorescent goo remains

We add 150ml water...

...and stir well to get all the actives absorbed by the water, scraping helps

All is now mixed. Note the brownish oily specks that won't dissolve in the water

After decanting the liquid (water), a brownish oily substance is left behind

 

[The Traveler]

Manske, salting!

Amount: Water 250ml, loads of salt (until saturated)

The water is cooked, salt is added until no more salt will be absorbed. Then the salt saturated water is added to the redissolved harmalas

To cool down the now 400ml of warm liquid I let it cool in the sink with cold water

When the liquid was cooled to room temperature harmalas already started to precipitate

The precipitation at room temperature

 

[The Traveler]

Filtering out the harmalas

Note: The container from the previous post was placed in the fridge. It was placed there in the evening at about 22:00 and the next day it was retrieved at about 14:00.

The container is fridgely cold and we see a nice precipitation

From the side

Pouring it all into a filter to catch the harmalas

The harmalas in the filter

The filter spread out, with the brownish 'mud' containing the harmalas

 

[The Traveler]

Redissolving the filtered harmalas in water and the addition of sodium carbonate

Amount: 200ml water, a few grams of sodium carbonate

The filter with the harmala mud on it is placed in the water

The harmalas dissolve easily into the water

The sodium carbonate is added and the solution is stirred well

Then suddenly we see precipitation!

Nice white flakes

At first the flakes float on top, but after a while they will drop to the bottom. A little shake now and then helps to hasten this process

 

[The Traveler]

Washing the harmalas

Amount: 500ml water per wash.

Note: We need to wash the harmalas to remove the salt and the sodium carbonate. To wash the harmalas we put them in a container filled with water, after the harmalas settled to the bottom we decant and discard the liquid. About three washes with 500ml water are more then enough to completely remove the salt and the sodium carbonate taste from the water.

Once the harmalas have settled at the bottom...

...the liquid can be decanted and discarded

The harmalas after the decantation!

We fill the container with water again

Tip of the trade: cut your PH-strips into smaller ones, this way you have (in my case at least) 4 times the amount of PH-strips

The ph is still too high after one wash

The harmalas however already look stunningly white

 

[The Traveler]

Drying the harmalas

We put the harmalas in the food dehydrator and dry it at 70C

The harmalas are now completely dried and ready to scrape up

 

[The Traveler]

Scraping it up and the (embarrassing) yield

Note: the yield is really low, just 0.3%. This is mostly due to only two pulls and the speed in which the pulls were made. The third pull is now soaking for over a day and will be processed soon to check it's yield.

All is scraped up into a nice sort of pyramid

And the embarrassing yield!



Any questions and remarks are welcome!

 

[neverwas]

Very interesting. It's nice to see people still experimenting with Rue extractions. I'm not keen enough with chemistry to develop my own process yet so it helps that other people are, gives me a chance to practice. Especially since My next extraction is from Rue whenever it arrives.

Keep us updated and good work!

 

[endlessness]

Awesome job trav! Thanks for taking the work to record and post this!

Maybe harmala phosphates arent very IPA-soluble and hence the low yield? keep pulling to see how much comes out.. Or when you' re bored of pulling, a normal A/B can be done on spent seeds to see if more comes off?

Another possibility is that the water+harmalas wasnt enough salt-saturated ? Maybe instead of adding salt-saturated water to the harmala solution, what about boiling the harmala solution and saturating it directly?

And back to the phosphates solubility, if one could weight the amount of evaporated phosphates and then try to dissolve in small amounts of fresh IPA, then we could know the solubility of the phosphates in IPA with numbers. Would be interesting also to do the same but extraction using IPA but with other acids to see what is ideal acid for this. Anyways many things we can test.. I love when people attempt different extractions

 

[gibran2]

Thanks for the time and effort put into this! (I know from personal experience how much time it can take.)

The yield sounds quite low – doesn’t rue often contain 5% or more alkaloids? Also, after recently reading about the “unwanted” alkaloids in rue – vasicine and vasicinone, I wonder if a Manske is really necessary? (Unless you’re a pregnant woman, it seems that vasicine and vasicinone actually have beneficial properties.)

There’s some discussion of this in this thread.

 

[The Traveler]

Maybe harmala phosphates arent very IPA-soluble and hence the low yield? keep pulling to see how much comes out.. Or when you' re bored of pulling, a normal A/B can be done on spent seeds to see if more comes off?

Another possibility is that the water+harmalas wasnt enough salt-saturated ? Maybe instead of adding salt-saturated water to the harmala solution, what about boiling the harmala solution and saturating it directly?

My guess is that harmala phosphates aren't very soluble in IPA.

After doing the manske and filtering out the harmalas I kept the filtered salty liquid, added a little water too it and then added sodium carbonate. I stirred it really well and NOTHING precipitated out of it. If there was any harmalas left in the liquid it should have precipitated out shouldn't it?

Thanks for the time and effort put into this! (I know from personal experience how much time it can take.)

The yield sounds quite low – doesn’t rue often contain 5% or more alkaloids?

I was thinking quite a lot about you and your write up while making my pictures and all. It's indeed a lot of work.

And yes, the yield is extremely low. I will keep pulling this but after say 5 pulls I will try pulling with water+phosphoric acid to see what still comes out of it.


Kind regards,

The Traveler

 

[Apoc]

Cool! So just wondering what is the phosphoric acid supposed to do? What if you just used IPA? This experiment also answered a question for me. It seems like the technique that Gibran2 performs in his easy caapi tek will work with syrian rue. That is, add base to harmalas, and you'll get precip.