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Best type of column chromatography for small quantities?

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69ron

69ron

Rising Star
Ok, so why is SWIM interested now? He’s been trying to crystallize bufotenine for many months now with no success. He’d tried everything with no luck. So now he wants to try column chromatography to separate the bufotenine from the amber material that’s stuck to it.

There’s more than one type of column chromatography. I’ve read a little about them and dry vacuum seems to be the best and cheapest, but having no experience, I can’t say for sure.


Which type of column chromatography do you think is best for small quantities (100 mg – 1 gram)?

A: Gravity column chromatography
B: Flash chromatography
C: Dry vacuum column chromatography (A.K.A., dry-column flash chromatography)


For dry vacuum column chromatography you need Merck grade 60 silica gel. Where can that be found? Is there a substitute silica gel that’s easy to get that could be used instead? I can find silica gel all over the place but most of it doesn’t give the grade or mesh size.
 
Why is flash chromatography better for small quantities than dry vacuum column chromatography?

Also, is there any advantage to using gravity column chromatography? Or is that obsolete?
 
benzyme said:
so the activated carbon didn't pan out? odd :?
Click to expand...

No...it absorbs all the bufotenine and the amber stuff and it's nearly impossible to get them out of the carbon. SWIM had to Soxhlet extract it out of the carbon for many hours. After that, he still could not get any of it to crystallize. The amber junk is messing it up.

Supposedly, the amber junk elutes as a brown oil before bufotenine elutes when separated via column chromatography. The only reason it’s amber is because the white bufotenine is mixed with it.
 
69ron said:
Why is flash chromatography better for small quantities than dry vacuum column chromatography?

Also, is there any advantage to using gravity column chromatography? Or is that obsolete?
Click to expand...

either/or for your first question (neither is really significantly advantageous over the other). both are quick and effective

and yah, gravity really is obsolete, but still useful if using a large quantity of known mixtures. it's really about how long one is willing to wait
 
Nearly all the successful attempts at crystallizing bufotenine I’ve read about were done only after separation via column chromatography. In all cases a brown oil elutes before the bufotenine does.

SWIM crystallized bufotenine using Ott’s method once without running a column, but he just got lucky. He’s since tried using Ott’s method with no luck. He’s tried dozens of times since using different tricks and can’t get it to crystallize even the slightest bit. There’s too much of the amber material present. SWIM has tried every solvent he has and all the solvents that bufotenine is soluble in, the amber material is also soluble in. Even precipitating bufotenine from acetone as the citrate doesn’t separate it from the amber material!

I think at this point the only thing that will help is running a column. SWIM wants to use the best possible method. He’s used gravity column chromatography before, but doesn’t have a column or silica anymore.

He’ll need to invest in new equipment and isn’t sure if he should go for gravity column chromatography, flash chromatography, or dry vacuum column chromatography.
 
benzyme said:
69ron said:
Why is flash chromatography better for small quantities than dry vacuum column chromatography?

Also, is there any advantage to using gravity column chromatography? Or is that obsolete?
Click to expand...

either/or for your first question (neither is really significantly advantageous over the other). both are quick and effective

and yah, gravity really is obsolete, but still useful if using a large quantity of known mixtures. it's really about how long one is willing to wait
Click to expand...

The faster the better, unless purity suffers?
 
Yeah...it boils at 320 C!

Vilca seeds really vary a lot in alkaloid content. The last batch SWIM extracted contains very little bufotenine and feels more toxic than usual. The alkaloid extract causes quite a bit of nausea, much more than usual. It’s unpleasant. It’s also barely visual at all, with the main effects being nausea for about 5 minutes and slightly prickly tingling sensations.

If Vilca was always like that, SWIM would hate Vilca with a passion. I don’t know which alkaloid is responsible for the toxic effects in this batch, but SWIM really wants to get the crap out. He’s got about 1 gram of this unpleasant alkaloid mix.

One thing he’s thought about doing is subjecting the extract to maybe 250 C for a while. That might cause the toxic stuff to vaporize away, leaving behind only the high boiling fractions like bufotenine.

The alkaloid profile in Vilca is actually much more complex than I was lead to believe by some authors. SWIM has had many alkaloid extracts made exactly the same way that have had very different levels of side effects and visual effects. Usually the experience begins with a little prickling sensation in the back of the head, and that’s followed by snake like visual effects making everything looks curvy and twisty, and then the visuals change to more DMT-like towards the end of the trip with the effects becoming quite euphoric. But with his latest batch the initial effects include very slight prickling, strong nausea, and then very weak visuals, and no euphoria at all. 10 mg is enough for very light closed eye visuals and some minor open eyed visuals and almost enough nausea for SWIM to feel like he’s about to vomit. Its very disappointing. The extract is also extremely sticky. 10 mg is usually enough for full blown visual effects causing objects to be seen hovering in front of you with your eyes open. But not with this batch. It’s very high in side effects and unpleasant.

The Vilca seeds SWIM purchased were from BBB and they were very tiny, the smallest he’s ever seen. He’s had good seeds from them before. SWIM is thinking its not Vilca but some other similar plant. It does have bufotenine in it, SWIM can feel it present, but it’s a minor alkaloid in terms of effects. They feel down right toxic.
 
SWIM would recommend flash chromatography over dry vacuum but its a cost issue. SWIM never does dry vacuum its most likely going to be less reproducible and dried silica makes a mess :shock: . However its cheaper to do dry vacuum and might be easier, if you are not used to column chromatography. Vacuums are cheaper and you can use very basic lab equipment to make a short stout column in a buchner funnel like set up. That will actually probably work nicely in SWIYs case.

Gravity will work but its not as efficient as flash chromatography because flash moves fast and can be under pressure so compounds don't spread out like they do with gravity columns.
 
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