CIELO - How to separate Mescaline Citrate from Other Alkaloids?

[highlightprotein]

Edit: This thread has now turned into my journal for my first extraction using CIELO. The posts regarding this start here.

The CIELO tek calls for salting with citric acid.

How can we separate mescaline citrate from the other alkaloids?

When using vinegar you can wash with MEK. When using HCL you can wash with acetone and IPA.

 

[Grey Fox]

Those are interesting experiments! I'm looking forward to hear about your results, especially regarding the yield from the core and white flesh.

There is no need to remove the clear skin. It doesn't harm the tea at all, and it should not affect your extraction. Additionally, I have always found that some green flesh is wasted when the clear skin is removed. Its almost impossible to remove all of the clear skin without some of the green flesh sticking to it and being lost. Its a tedious, wasteful, unnecessary step IMO.

 

[highlightprotein]

Yes I agree, when I was removing the waxy skin I saw some green stuff also get pulled off. Unless the waxy skin some how decreases the success rate of the extraction I don't think it was worth the effort. For example I weighed the waxy skin and it only came to about 10g wet for a bit less than half of my cactus- so this 10g wouldn't result in wasting too much CaOH/ethyl acetate/citric acid.

It's been about 12 hours in the dehydrator at 95F so far and I am surprised to see how much everything shrank! It seems pretty dry but I think I'll wait until the 24 hour mark to be sure.

 

[highlightprotein]

Ouch, after 24 hours in the dehydrator, I only had about 70g of material, from 18" of cactus. I was expecting much more than this. I decided to abandon my experiment and just combine them all. Perhaps next time I will buy a much larger cactus and retry.

Moreover, while I thought that my cactus stars were totally dry, after putting them in the blender I discovered that this was not true. It made the blending more difficult than necessary and it seems I lost a bunch of powder to the blender because of this. I have transferred the powder/chunks back to the dehydrator.

I think next time I will slice up my stars into much smaller pieces and then place the small pieces in the dehydrator instead of putting the stars directly into the dehydrator. Also the waxy skin does not seem to want to be pulverized in the blender. I'm hoping that this is due to it being too wet and not due to some intrinsic quality of the waxy skin.

 

[highlightprotein]

Double ouch: after another 12 hours in the dehydrator, I was left with about 39g ! Edit: I don't think the waxy skin is difficult to pulverize in the blender, so long as it is totally dry. Next time I will just cut the stars into very tiny pieces before putting in the dehydrator, and potentially dry it out for 36 hours instead of 24.

I made the 69ron paste without issue, and then microwaved it. I noticed some browning, and also the microwave seemed to cause a lot of the material to form into little balls/clumps. I hope this doesn't block the EA from extracting.

I've placed the material in the fridge and the EA in the freezer. One concern I have is whether it is OK to let all this freebase mescaline sit around for 24 hours. Doesn't it readily react with air to form some kind of carbonate?

Hopefully I get some precipitation tomorrow.

Does anyone know if I can put the coffee filter + precipitate in a dehydrator? I'm not sure if the evaporating EA might cause some kind of harm to the dehydrator. If I just leave it out on the counter, about how long will it take to evaporate?

 

[_Trip_]

If the paste is based and you haven't over microwaved it (as in evaporated too much water out-2/3rds is normally a good number as per TEK) then the EA should extract the alkaloids fine. Having it based for 24hours wont change your yields, I believe Loveall and maybe Shroombee tested this with no noticeable difference.

I'm guessing you used sodium carbonate as a base? not calcium hydroxide? I believe it should be fine either way, I don't think the carbonate reacts and affects yields.

You don't have to use a coffee filter to catch the crystals (I always lose product when using coffee filters). You need to filter the EA after the pulls to get the gunk out but the precipitate mescaline citrate is usually very sticky. So another option is that you should be able to decant the EA if you are careful while the mesc citrate sticks to the walls of the jar. For me this works best when using more citrate and giving it a good shake to fast track precipitation.
Anyway, decant and leave the mesc citrate that's in the jar to dry, then you can add a tiny amount of water until the mesc citrate is all dissolved (shake the jar). Pour out the water into a dish to evaporate. Scrape it up and you're done.

To answer your question the crystals have a tendency to stick when drying so it may be alright in a dehydrator but i think a bit of product may get stuck in the filter (a small amount potentially could get blown away). You could always wash the filter in water and evaporate it to get the mesc citrate out of the filter too.

Anyway that's my opinion.

 

[downwardsfromzero]

I've placed the material in the fridge and the EA in the freezer. One concern I have is whether it is OK to let all this freebase mescaline sit around for 24 hours. Doesn't it readily react with air to form some kind of carbonate?

You will surely have kept your EA/mesc solution in a tightly stoppered container? It will make the entire contents of your fridge and freezer stink if the vessel is open. Butyl acetate made my ice cream turn banana flavoured, even though it was in a closed jam jar at the bottom of the freezer and the ice cream was in another compartment 1m higher. Also, the solvent will absorb water and you'll get a bunch of ice crystals potentially messing up your processes (e.g., formation of citrate crystals). In the fridge, especially, but also in the freezer - albeit far more slowly - the solvent will gradually evaporate (think of where that odour is coming from) and only then will you eventually be left with a soggy puddle of mescaline autocarbamate/carbonate.

You could try crystallising out mescaline carbonate using a soda stream, just for the lulz. It's a viable technique to use carbonated water for backsalting of mesc from a NPS. I would suggest that carbonating ethyl acetate might require some forethought, principally in matters of compatibility of plastic components.

 

[highlightprotein]

You will surely have kept your EA/mesc solution in a tightly stoppered container?

I hope I read the tek correctly. What I did is make just the 69ron paste (cacti + water + CaOH), without any EA at this point, and then placed the bowl in a ziplock inside of my refrigerator. I separately placed pure EA in my freezer (in a mason jar- I hope the food in my freezer isn't ruined!). I then waited 24 hours, took them both out, and started the extraction.

Cold extract option: With this option the paste is cooled in the fridge and fresh ethyl acetate is chilled in the freezer (if using reused solvent filter ice crystals from freezer) for 24h or more. The extraction time per pull is cut down to 60 seconds. The shorter pull time minimizes plant material (such as chlorophyl) in the extract, which we believe helps with crystalization. While a colder extract could theoretically lower the yield, experimentally the yield was ok

Was I supposed to have performed the extraction at room temperature and then let the EA/mesc settle in the freezer for 24 hours?

 

[highlightprotein]

Some notes on my extraction phase:

I ordered a stainless steel french press online but unfortunately it was missing all of the filters, rendering it useless. I ended up purchasing a glass french press with a single plastic piece at a local store. This was a mistake because I had to awkwardly hold the plastic piece out of the way when I poured off the EA. I was able to do it without any issue, but it just made everything more difficult.

Edit: Actually I just re-checked the picture in the CIELO tek, where a french press with a plastic piece is being used. Is it reasonable to conclude that plastic used in french press is HDPE? The plastic piece on my french press doesn't indicate what kind of plastic it is.

The first pull was entirely swallowed up by the 69ron paste. I first thought I made some mistake. However the second pull was liquidy and I was able to filter it easily.

Pouring the EA/mesc out of the french press and through a coffee filter worked fine for about 80-90% of the solution. However the last 20% seemed to get stuck in the filter. I just grabbed another filter and dumped the first filter into it. But in total I went through 12 filters. These filters are all now green and smell like EA which makes me concerned about throwing them in the trash.. I think it might be better to invest in some lab grade filters in the future.

I also lost about 20% of my solvent to the 69ron paste. Is that normal or will it affect my yields by 20%?

Right now I'm waiting the 1 hour to see if there is any droplets or particles. At least right now I do not see any water droplets/particles. When I shine a flashlight through the solution it appears pretty light green.

I'm going to try the fast crystalization method with 10mg (edit: I'll do 15mg instead of 10mg) of citric acid per gram of EA on my stir plate. I'll report back in an hour or so. Wish me luck!

I'm guessing you used sodium carbonate as a base? not calcium hydroxide?

I used CaOH.

So another option is that you should be able to decant the EA if you are careful while the mesc citrate sticks to the walls of the jar...Anyway, decant and leave the mesc citrate that's in the jar to dry, then you can add a tiny amount of water until the mesc citrate is all dissolved (shake the jar). Pour out the water into a dish to evaporate. Scrape it up and you're done.

I'll keep it in mind, thanks. For now I will dump it through the filter just because I want to try to follow the tek exactly. But I'll collect it in another jar and let it settle and if I see any crystals I will try your decanting method.

 

[highlightprotein]

After waiting 1 hour, the solution looked very clean: no sediment or water drops that I could see.

I added 15mg citric acid per gram of EA. The solution immediately turned very cloudy, which was promising.

I put it on my stir plate at a high speed. After 8-10 minutes I took it off the stir plate (was this enough time?) and saw what I thought were crystals stuck on one side of the bottom of the jar. However, I noticed I could not really kick the crystals up when shaking the container. I shook some more, and then wondered if I didn't really see any crystals, because what I basically saw after shaking manually was some kind of yellow/brownish goo that sticks to the jar and is hard to move.

Too bad! I recall reading in the CIELO thread a few people ran into this problem and couldn't resolve it. I hope that is not the case here... I put it back on the stir plate and waited about 20 minutes but nothing changed.

I filtered the EA through the coffee filter and basically couldn't get any precipitate to come through (I did get a small chunk of some brownish stuff in the filter. It never really dried even with a fan for 30 minutes, and I ended up losing this chunk to the filter). I washed the vessel with fresh EA 3 more times and it was totally clear colored after filtering. I took all of the filtered EA and just for kicks added enough citric acid to make 20mg per gram of EA, but didn't see any cloudiness at all. I put it on my stir plate for 10 minutes and saw nothing, no goo and no crystals. So it seems my original citric acid reacted completed.

I'm going to wait for the remaining EA to evaporate from my vessel with the goo in it, and then add some DH20 and see what happens. Hopefully the goo will dissolve and then I can evaporate it and rewash with EA.

Edit: I washed the goo with DH2O and filtered through a coffee filter but didn't see anything get stuck in the filter. I'm now evaporating it on a dish in my food dehydrator at 160F.

Does anyone have any suggestions for handling this goo stuff? I need to go back and re-read the CEILO thread because I forgot how this issue was resolved.

 

[Loveall]

I'm going to wait for the remaining EA to evaporate from my vessel with the goo in it, and then add some DH20 and see what happens. Hopefully the goo will dissolve and then I can evaporate it and rewash with EA.

Does anyone have any suggestions for handling this goo stuff? I need to go back and re-read the CEILO thread because I forgot how this issue was resolved.

Sometimes people don't get crystals, but the goo should be where the product is at. What options did you use for the cielo Tek? Microwave and cold solvent seem to give the largest xtals. I also wanna try washing the extract with brine before salting with citric.

Use warm water/hot to dissolve the goo. It may take a while, give it time. Them evaporate slowly, you will likely get something xtaline and relatively pure.

 

[downwardsfromzero]

I ended up purchasing a glass french press with a single plastic piece at a local store. This was a mistake because I had to awkwardly hold the plastic piece out of the way when I poured off the EA. I was able to do it without any issue, but it just made everything more difficult

On all the French presses I've seen that have a plastic insert inside a metal lid the insert is held in place with a nut. It should be possible to dismantle the entire thing in order to remove the plastic piece. Of course, yours may be glued or injection moulded or whatever so in that case you'd have to just carry on as before.

 

[highlightprotein]

What options did you use for the cielo Tek? Microwave and cold solvent seem to give the largest xtals. I also wanna try washing the extract with brine before salting with citric.

I used Bridgesii cactus, and I used the following options: microwave, cold EA, and fast crystallization with 15mg citric acid per gram of EA. Next time I might try some pachanoi and/or slow crystallization.

Do you know if there is a simple way to wash the goo to get some nice crystals? For example, has anyone tested mescaline citrate's solubility in acetone, 99% IPA, etc? I will use the goo if there is no other option but I would love to have some nice crystals.

I would rather not subject this goo to an A/B as I would like to avoid working with lye and HCl if possible.

Thanks!

 

[highlightprotein]

After putting this evaporated goo in my food dehydrator at 165F, it resulted in what appeared to be some similar brown looking goo on my plate. I was disappointed until I started chinking away at it with a razor blade, where I discovered that it was crystalline.

However, it is so sticky, and rather hard. I have lost a lot of material going at it with the razor blade. In fact a piece actually landed in my eye which freaked me out. I washed it out for like 3 minutes and returned back and started using eye protection. (Edit: it's been about 3 hours since this incident. My eye feels fine. I hope it stays that way; edit: It's now been over 12 hours and I am fine.)

I took it out of my food dehydrator and let it cool down for about an hour before I started scraping it. Was this a mistake? Perhaps it would have been easier if I started scraping it immediately after taking it out of the food dehydrator.

So far, I have yielded about 1.1g of brown crystals, whereas I started with about 39g of dried cactus material. So this is a yield of 2.8%. And this doesn't include all the loss I've had just scraping it with my razor blade. I see brown crystals on the floor and the counter and my shirt. But 2.8% is too good to be true right? I assume that implies my brown crystals are not as pure as could be.

I also used a regular ceramic plate instead of a glass evap dish. I now have scratch marks all over that plate. I hope it doesn't mean that my 1.1g of brown crystals contains some plate material! Although, that might explain the higher than expected yield . None of the glass dishes I saw at Walmart were thin enough to fit inside of my food dehydrator. Next time I'll go buy something better online for this.

Edit: I ended up adding some boiling water to this plate to dissolve the crystals I couldn't get out and then put it back in the dehydrator. After it evaporated I took it out and immediately started scraping. This seemed to be easier compared to scraping after it had cooled down. But it wasn't that much easier. I think these brown crystals that originate from the goo just have a tendency to become pretty hard and sticky, and difficult to work with.

 

[shroombee]

None of the glass dishes I saw at Walmart were thin enough to fit inside of my food dehydrator. Next time I'll go buy something better online for this.

I use these plates in my dehydrator. Not perfect because they have a minor recess around the perimeter, but good enough. I'm able to use a razor blade to scrape probably 95% of evaporated product with just a little remaining at the corners.

https://www.amazon.com/gp/product/B088ZSG43G?th=1

 

[highlightprotein]

I use these plates in my dehydrator. Not perfect because they have a minor recess around the perimeter, but good enough. I'm able to use a razor blade to scrape probably 95% of evaporated product with just a little remaining at the corners.

https://www.amazon.com/gp/product/B088ZSG43G?th=1

Thanks, I will get these for next time.

Shroombee, if I remember correctly from the CIELO thread, you also ran into some problems with the getting goo/brown crystals.

Did you figure out a way to resolve this? I used the microwave, chilled EA, and fast crystallization with 15mg citric acid per gram of EA on a stir plate on some Bridgessi cactus. However I got this yellow/brown goo that turned into brown, sticky, crystals. It would be great if I could get some nice white crystals that were not so sticky.

 

[highlightprotein]

Ok this is a bit weird: I did a 7th pull with room temp EA which yielded white crystals, no goo.

Yesterday night, several hours after starting the original extraction, I decided to do a 7th pull with a large quantity of fresh, room temperature EA. I mixed the EA and the 69ron paste vigorously (whereas the previous pulls I did not mix vigorously), and let it sit for about 5 minutes (compared to just 1 minute with the previous cold extractions). I then filtered it and put it in its own container (separate from the other 6 pulls), and added 15mg citric acid per gram of EA. I saw it turn cloudy immediately and thought that was kind of unexpected since there should be nothing active in the 7th pull. I set it on my stir plate at a high speed for 10 minutes but didn't see any crystals at all, which made sense.

However, I left the EA out and just checked it this morning. There appears to be a large amount of beautiful white crystals! And no brown/yellow goo at all! I'm going to let it sit for another 8 hours before filtering and weighing it.

It is confusing on three accounts: 1) why am I still getting yield from a 7th pull, 2) why is it yielding beautiful white crystals but no goo?? 3) Why did I have to wait 12-18 hours before seeing crystals form when I did the fast crystallization on a stir plate with 15mg citric acid per gram of EA?

It makes me wonder if next time I should put each pull in its own container and salt them separately. Perhaps the earlier pulls are grabbing some compound that is resulting in the goo. But I still don't get why I'm still getting yield after 7 pulls. I wonder if the cold extraction plus the short extraction times may result in some kind of loss in yield (although the tek says it shouldn't be the case). At least for me, the cold extraction/short extraction times did not help avoiding the goo problem. My 7th pull was room temp EA shaken vigorously with a long extraction time which successfully yielded beautiful white crystals.

 

[shroombee]

Shroombee, if I remember correctly from the CIELO thread, you also ran into some problems with the getting goo/brown crystals.

I didn't have the goo results. My first run or two were experimental where I didn't get xtals to crash. We eventually figured out the process of adding a lot of excess citric and stirring vigorously to get the xtals to crash quickly.

Ok this is a bit weird: I did a 7th pull with room temp EA which yielded white crystals, no goo.

This is very interesting and unexpected. Let's see what you have after filtering and weighing.

 

[downwardsfromzero]

1) why am I still getting yield from a 7th pull

Some cactus simply takes longer to break down and release the alkaloids, it seems. (Many moons ago, I did a q21q21 on some material of uncertain origin and the first pulls yielded practically nothing. The mixture was abandoned for several weeks and left to dry out. Later, after adding more lime and water, a few more pulls ended up yielding a usable amount of product.)

 

[highlightprotein]

My 7th pull resulted in 0.24g of easy to scrape crystals (from an original 39g of cacti, and I already extracted 1.1g of brown crystals from the goo). However they were not beautiful white crystals- they looked white in the EA solution, but after decanting/evaporating it resulted in a mix of light brown and light yellow crystals.

After decanting this 7th pull, I could visually see a mixture of white crystals and yellow crystals (while it was in solution, it appeared to be totally white crystals). I added some fresh EA and swirled it around and decanted, three times. I noticed that the yellow crystals were much more likely to be disturbed by the EA wash, while the white crystals seemed to ignore it and just stick to the walls. On the third time I swirled hard and immediately poured it all out through a coffee filter. That coffee filter contained predominately yellow crystals, while the white crystals were predominantly stuck in the vessel.

I dried the coffee filter and the crystals turned light brown. I got 0.18g from this. They were not sticky or hard at all- it was very easy to scrape and move around, unlike the previous brown crystals I got from scraping up the goo.

I added water to the vessel until all white crystals were dissolved, and evaporated in a food dehydrator at 165F. This resulted in 0.06g of light yellow crystals which were easy to scrape and not sticky.

In summary, my 7th pull seemed to be better- no goo, and the crystals were easy to scrape and move around; they were not hard and sticky like before. They were also lighter in color, ranging from light yellow to light brown.

I guess I will bioassay the light yellow crystals first, then the light brown crystals, and finally the dark brown crystals from the original 6 pulls/goo. Unfortunately I'll need a week or two before I can bioassay.

 

[Loveall]

Sounds good. Keep in mind that 100mg can be threshold for mescaline. Also, we think the process crashes the mono-mescaline citrate salt, which is ~60% as dense as mescaline HCl.