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Ion Exchange Resins: Experimental Design questions Options
 
Samvidbuho
#1 Posted : 10/1/2019 7:01:06 AM

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Hello esteemed community:


I’ve been wanting to try out some ion exchange resins for upcoming product isolation, but haven’t pushed myself to actually experiment with this yet. At the moment I’m planning a DOE, but since this would be my first go I was hoping somebody more knowledgeable than me could check it and provide some constructive feedback if applicable.


Initial thoughts: (Starting materials: MHRB)


Begin with standard A/B. After the acidification stage is complete,

Immerse: 1 teabag full of Amberlite IRC-50 ion exchange resin (WCX) and 1 teabag full of Amberlite IRA-67 ion exchange resin (WAX). Soak overnight.

Elute the teabag containing the IRC-50 with basified water, then extract with organic.


I think it really is this simple, but also…
is it really this simple??



Appreciation in advance !

 

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benzyme
#2 Posted : 10/1/2019 1:56:17 PM

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SCX would be more effective, for the separation of most alkaloids. ex. IR-120
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
Loveall
#3 Posted : 10/2/2019 1:13:31 AM

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It works, I've gotten DMT out of a cation resin. Pretty straight forward but not worth it I think since DMT separates/extracts so well already.

I added some salt during the basic elution, would recommend you consider the same.

Also, (in general) target the pH so it is not too low (two units below the pKa should be good). Same thing for elution pH, this reduces the ammount of proteins that come through (not usually a concern for DMT though). Also with enough salt you can elute at any pH and basify later.

I used a mason jar and a nylon filter sheet (from a hop beer brewing bag) that could go over the jar and be secured by he screw-on lid ring. This allows for quick rinsing with water until it runs clear before elution.

I think resins more interesting for the more difficult extractions with zwitterions like psiloc(yb)in or Harmalol.

Cheers and good luck.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-XπŸ’šπŸƒπŸ’š
 
Samvidbuho
#4 Posted : 10/2/2019 4:27:55 AM

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Thanks for both of your replies Very happy

Benzyme, would there be a functional difference between IR-120 and Dowex-50? (If Dowex is good, does the styrene-DVB % cross-linking make a difference or is that negligible?)

Loveall, so you wouldn't recommend doing this? The advantages of IEX I thought were enhanced extraction efficiency and a much shorter overall process, but honestly I have just been looking for something new to do / expand my skillset and such. I can see how it would be straightforward though -- not much room for any 'art', and I suppose it does seem a little dull.

The other route I might explore the role of surfactants in the extraction process..

Thank you for the tips, I'm sure I'll end up trying this at some point anyway down the road so this is great to have. Cheers
 
Loveall
#5 Posted : 10/2/2019 4:45:42 AM

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I did it and it was fun. I couldn't find an advantage for DMT, maybe you will.

One thing that surprised me is how difficult it is to elute these resins in practice. The expectations I had from reading were just off, that's all. I ended up making a very simple column with a simple vinyl tube from the hardware store instead of doing a batch process because of wanting to force elution better.

It was surprising to me how well the resin grabs on to stuff.

One thing I wish I would have done differently is start with bulk tryptophan from the supplement store to learn hands-on how the resin behaves without waisting mushrooms.

Good luck!
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-XπŸ’šπŸƒπŸ’š
 
Samvidbuho
#6 Posted : 10/2/2019 7:00:42 AM

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I get that.. 'practice reactions' would have been much more economical for me too historically speaking..

I did some wee tests with the resins a few months ago and thought I did have some success in just letting the exchanged resin equilibrate overnight into some basic water, no column - the column just speeds it up, no?

Think you sold me that this would be a fun thing to try then.. Much obliged


P.S. Since you like the interesting and complex,, have you ever experimented with reactive extraction techniques? I'm just getting into them now but I wonder if something clever could be done using, I dunno, an ion exchange resin for some sort of interfacial reaction with your zwitterions, pulling them into the organic then having the resin crash out with another ion exchange? (Eesh, maybe that wouldn't make sense, but something might..)
 
Loveall
#7 Posted : 10/2/2019 12:24:12 PM

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It does several things I think. I mentioned better elution. A front forms on it and compounds come out in an ordered fashion if things are setup right and technique is good. This could matter if proteins and other stuff we don't want are around.

See below for a picture of my setup. It is very easy. Tube was only a few bucks at the hardware store and the bottom is simply a nylon hop bag held in place by a strong rubber band. The top is just stuffed polyfill (pillow stuffing) to keep the top of the resin in place (it will also filter dirt particles).
Loveall attached the following image(s):
IMG_20190826_174408616.jpg (2,672kb) downloaded 51 time(s).
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-XπŸ’šπŸƒπŸ’š
 
benzyme
#8 Posted : 10/2/2019 2:13:03 PM

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Samvidbuho wrote:
Benzyme, would there be a functional difference between IR-120 and Dowex-50? (If Dowex is good, does the styrene-DVB % cross-linking make a difference or is that negligible?)


depends on the analyte(s) you're trying to separate. I retract my previous reply..IR-120 would be better at separating ergolines from mg seeds, fungus, etc.
but Dowex-50 is suitable for what you're trying to do. The higher %age crosslinking is geared more towards analytes with more side-chains, and proton acceptors/donors.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
Samvidbuho
#9 Posted : 10/3/2019 3:03:59 AM

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Dazzling...

Thank you both immensely, great help
 
 
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