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Low yield on rue extraction Options
 
moyshekapoyre
#1 Posted : 7/19/2014 3:24:20 AM
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I've just finished the many acid/base extractions on this 45g of 10x rue powder I have. I should have ended up with about 20-25g of pure harmalas (since bioassay indicates the 10x rue is about half alks), but instead it looks like only a few grams, so I'm kinda sad about that.

Clearly there is something amiss in my technique, but I can't pinpoint it. I thought I was waiting quite a good while between each pull so that things could settle out of solution (like a day or two each time). But I only waited about 5 hours maybe to cool the manske liquid, so perhaps that was the problem. The liquid was still colored like it had some harmalas. D'oh! Next time I guess I'll leave it in there for a few days?

And perhaps I didn't use enough water? It was only maybe 800mL, but I felt that that should have been more than enough to dissolve 20-25g of harmalas.
 

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TreehouseChemist
#2 Posted : 7/19/2014 6:47:18 AM

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Not to contend with your bioassay, but I think mathematically you were a bit optimistic. From my experience, rue extractions yield about 2-4% alkaloids by seed weight.

45g * 10x extract = 450g of seeds worth of alkaloids

450g seeds * .02-.04 = 9-18g of alkaloids

Plus, in addition to any lost during this extraction session, when it was extracted originally and made in to a 10x extract there could have been some loss. Subtract that from the expected yield too.

So you may not have wasted as much as you think, but you probably did toss a little on the Manske. Crystals can keep growing for 8-10 hours after hitting room temperature (24hr for 2+L solutions).

What was your extraction procedure like? Could use a few details Razz
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moyshekapoyre
#3 Posted : 7/19/2014 11:48:50 AM
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Thanks for the response. So 24 hours is always sufficient time in the fridge for manske?

My procedure was simply acid/base extraction repeated maybe 5 times. I basified with sodium carbonate until the solution felt soapy, left it in fridge for a day or two, filtered out the sediment and then redissolving that sediment in pH 1 water and then leaving that out for a day or two, then filtering and trashing that sediment, and so on. Then the manske step where I boiled it up and added non-iodized salt until no more would dissolve and you know the rest.
 
Jees
#4 Posted : 7/19/2014 1:44:21 PM

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* For manske your solution is better to be somewhat concentrated, if the volume is too large, the crystals grow more difficult. Did 1 liter for 100 gr of seeds.

* Amount of salt: I go for 20gr per 100 ml of solution, it is high but it still delivers very long needles, and I have no pesky salt contamination. Phosphoric acid was used at pH 3.

* This batch of 100 gr seeds delivered 5.44 gr, good for 4.6 freebase grams, personal lowest yield ever, still okay in general.

* When the solution comes from the stove, before it gets cooled it goes trough a very fine coffee filter. It is weird to catch a lot of dust in that phase, probably added (anti clogging?) agents from the salt?

* It takes a lot of effort to get all actives out of seeds, actually I have to powder them to get them. Sticking with whole seeds never got me good results for some reason.

* YMMV.

Fine gold:
Jees attached the following image(s):
Rue.HCL.jpg (363kb) downloaded 329 time(s).
 
tgun
#5 Posted : 8/10/2014 8:42:16 PM

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I had some cloudiness remaining in liquid and I just added a bit more lye solution and it crashed right out. I followed the easy caapi tek by gibran2. You could do a Manske on it after, if you wanted to. He states he did it with rue and as did I but I didnt bother with manske as it was good as is. He lost a certain % doing a Manske but it is apparently still a good yield for doing so. Not sure why you got an extract then extracted but it would likely be much more less costly using seeds. If that matters?
 
MelCat
#6 Posted : 8/10/2014 9:31:42 PM

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Jees wrote:
* This batch of 100 gr seeds delivered 5.44 gr, good for 4.6 freebase grams, personal lowest yield ever, still okay in general.

Fine gold:


Beautiful results! I love looking at those manske'd needles. Love
Convert a melodic element into a rhythmic element...
 
Jees
#7 Posted : 8/19/2014 6:28:13 PM

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Thx Melcat, makes me happy to share these feelings about our passion Wink
 
MelCat
#8 Posted : 8/20/2014 3:13:13 AM

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Jees wrote:
* For manske your solution is better to be somewhat concentrated, if the volume is too large, the crystals grow more difficult. Did 1 liter for 100 gr of seeds.

* Amount of salt: I go for 20gr per 100 ml of solution, it is high but it still delivers very long needles, and I have no pesky salt contamination. Phosphoric acid was used at pH 3.

* This batch of 100 gr seeds delivered 5.44 gr, good for 4.6 freebase grams, personal lowest yield ever, still okay in general.

* When the solution comes from the stove, before it gets cooled it goes trough a very fine coffee filter. It is weird to catch a lot of dust in that phase, probably added (anti clogging?) agents from the salt?

* It takes a lot of effort to get all actives out of seeds, actually I have to powder them to get them. Sticking with whole seeds never got me good results for some reason.

* YMMV.

Fine gold:


I added some of your tips to the Tao of Rue wiki page.
Convert a melodic element into a rhythmic element...
 
Jees
#9 Posted : 10/3/2014 10:17:20 PM

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Jees wrote:
* For manske... I go for 20gr per 100 ml of solution, it is high but it still delivers very long needles, and I have no pesky salt contamination....

Recently got another brand of salt and had to decrease to 10 gr per 100 ml to get same results on salt contamination**, no way I could use 20 with this new salt. No clue why it made such a difference, both stated NaCl table salt with some anti clogging agent.

** the point where the dry needles have no salty taste.
 
GreenDMT
#10 Posted : 7/22/2017 5:31:46 PM

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I have a little problem about 10x,maybe you encountered about it. I've put in a pot with acetic acid and boiled, after filtered and based and nothing precipitated, it's very strange, I've put a lot of base and nothing happened. What do you think is the problem?
Thanks
 
ShamensStamen
#11 Posted : 7/22/2017 9:15:58 PM
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Most people i've come across have never had good success with using 10x Rue extract, i'm not sure why but i personally would recommend boiling up about 100 grams or so of whole Rue seed a few good times, filtering it, reducing the boils down to about 400mls, once it cools to room temp add about 75mls of vinegar, dissolve 15 to 20 grams of washing soda into 100mls of hot water and pour/stir the washing soda water into the main brew, which will precipitate out the full spectrum crude extract, which can then be cleaned up a few times by filtering out the extract, re-dissolving it in fresh warm vinegar water (75mls of vinegar, 300 to 400mls of warm water), and once it's re-dissolved, filter out the black/brown plant gunk, and re-base the liquid, clean it up a few more times by re-dissolving it, re-filtering it, and re-basing it, and then filter it out and let it dry. Once dry, it's ready to go.
 
GreenDMT
#12 Posted : 7/22/2017 9:20:28 PM

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I didn't have seeds,I extracted from seeds, but this 10x is far away from my expectation...now I'm in a phase of not precipitation by adding base, and I don't know that to do next, adding more base or...

ShamensStamen wrote:
Most people i've come across have never had good success with using 10x Rue extract, i'm not sure why but i personally would recommend boiling up about 100 grams or so of whole Rue seed a few good times, filtering it, reducing the boils down to about 400mls, once it cools to room temp add about 75mls of vinegar, dissolve 15 to 20 grams of washing soda into 100mls of hot water and pour/stir the washing soda water into the main brew, which will precipitate out the full spectrum crude extract, which can then be cleaned up a few times by filtering out the extract, re-dissolving it in fresh warm vinegar water (75mls of vinegar, 300 to 400mls of warm water), and once it's re-dissolved, filter out the black/brown plant gunk, and re-base the liquid, clean it up a few more times by re-dissolving it, re-filtering it, and re-basing it, and then filter it out and let it dry. Once dry, it's ready to go.

 
ShamensStamen
#13 Posted : 7/22/2017 9:43:18 PM
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How concentrated is the brew? How much acid did you use? Are you sure you used enough base to counteract the acidity and raise the pH up enough to precipitate out the alkaloids? If you did, then idk, maybe the 10x extract just isn't good. A lot of people don't like the 10x extract, and idk how much alkaloids are in 10x extract but people don't seem to have good luck with it. I'd say just stick to boiling seeds and making your own extracts, or find some freebased or hcl extracts online.
 
GreenDMT
#14 Posted : 7/22/2017 10:09:41 PM

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I ended with 400 ml of brew with a little of acetic 20-40 ml then added like 30 g of base, nothing happened, I will put more base, but after it I don't know how to recover
ShamensStamen wrote:
How concentrated is the brew? How much acid did you use? Are you sure you used enough base to counteract the acidity and raise the pH up enough to precipitate out the alkaloids? If you did, then idk, maybe the 10x extract just isn't good. A lot of people don't like the 10x extract, and idk how much alkaloids are in 10x extract but people don't seem to have good luck with it. I'd say just stick to boiling seeds and making your own extracts, or find some freebased or hcl extracts online.

 
ShamensStamen
#15 Posted : 7/23/2017 12:12:33 AM
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Well it sounds like you did it right, perhaps your 10x extract is just bunk, which is actually quite common from what i've read. I'd say, stick to seeds or homemade extracts.
 
GreenDMT
#16 Posted : 7/23/2017 2:27:56 PM

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Thanks for reply, I will consider that in the future.
 
blue.magic
#17 Posted : 7/23/2017 3:42:01 PM

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Once you filter out harmala crystals, try to basify the water. You may be suprised how much harmala freebase precipitated. You can than redissolve the recovered freebase in hot vinegar and do a separate Manske, or combine the two harmala.HCl solutions.

My last extraction from rue yielded over 2.1% when recovering the unprecipitated harmalas.

I also tried lab-grade salt (99.98% NaCl) + DI water and found harmalas crystallize very quickly for 10 g/100 mL salt concentration, so even less salt would not harm if you have pure salt.
 
 
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