Trying to rescue acetone extract goo with ethyl acetate - no precipitation

[plantatron]

Hi Nexians,

I have a question about how to be rescue a cactus extract that was made in haste a couple of years ago.

Due to needing to move, several cacti couldn't be transported and so an extraction was attempted.

Experiments using limonene 69ron-style yielded some goo that couldn't be precisely dosed, and there was no time to dry all the cactus.

Thus, the idea was to extract with Acetone and precipitate mescaline sulfate.

The method was roughly as follows:

• freeze cactus
• cook in water, multiple times
• reduce liquid by boiling down
• add copious amounts of calcium hydroxide to the liquid and dry it with a heat bath
• the dried cactus+lime extract powder was then pulled with acetone
• there was no pure sulfuric acid possible to procure, so "aquarium pH down" was used

Unfortunately, nothing precipitated. Adding more pH down eventually precipitated something, but adding more, precipitated more and the product didn't seem like mescaline.

So in time stress, the acetone was evaporated, leaving a gooey orange-grey product that did smell strongly of acetone even after weeks. Not exactly food grade. This stuff then sat around for a couple of years.

Now, with the fairly recent advancements using ethyl acetate, the idea was to extract that goo with EA.

The extract showed to be strongly acidic, so the method used so far was:

• saturate distilled water with calcium hydroxide
• mix extract goo with small amount of that lime water, heat in water bath until all is dissolved (no issue here)
• pH paper showed the solution to be strongly basic
• continue heating until all the water has evaporated
• break residue into powder
• pull powder with EA
• no water droplets were apparent after decanting through coffee filter
• salt with citric acid

So far so good. Adding the citric acid clouded the solution like shown in the CIELO animation. The solution was left alone for 3 days and it looked like something had precipitated.

After decanting, though, the amount of precipitate was found to be extremely low. It was like a fine layer of "oily glue" on the glas wall that yielded very little when scraped plus some very small orangey flakes.

TLC revealed that the precipitate is not mescaline and all the mescaline is still in the EA solution.

So, now my question is: what to make of this and how to proceed?

Unfortunately, the citric acid wasn't weighted, the experiment above was a small scale test, about a teaspoon of citric acid powder was added to 50ml of EA. Should simply more citric acid be added?

Is it possible that the sulfate wasn't fully bound/removed by the calcium hydroxide step and is now interfering with the citrate?

Can it be cleaned somehow?

Any pointers would be super helpful and appreciated.

 

[modern]

Use sodium carbonate to make it alkaline it's easier to work with when not dry tek. I've done extractions from tea with calcium hydroxide and it is always a mess when larger amounts of water is involved.

The goo likely means your ethyl acetate was too wet. You can do a fridge rest but I found best way is using sodium carbonate to dry adding until it doesn't clump.... you can't add too much sodium carbonate IME so far. Needed more soda ash then tek says but I do liquid liquid extraction so makes sense.

 

[modern]

So apparently you can add too much sodium carbonate. I had a precipitate that wasn't mescaline citrate but most likely sodium citrate. Loveall mentioned it is likely from a buffer formed formed. I'm gonna end up abandoning ethyl acetate as the solvent and only use it for clean ups.

I've done a few extractions without issues of sodium citrate but I think I would need to distill the solvent quite often. With the lime it'll prevent this issue unless calcium citrate also precipitates?

I'm gonna need to start my data collecting from scratch since I think all my mescaline citrate extractions have been contaminated so results are likely off.