San Pedro Alcohol Extraction Acids & Bases in alcohol pulls

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This thread is largely to satisfy my own curiosity & help me understand some of the chemistry behind what I've seen in a recent extraction.

I started off using ethanol to extract some san pedro powder, after a few days soaking it yielded a very dark ethanol, I evaped this off to get a thick dark browny black resin. Great.

Then prompted by another post here I decided to try the next round with a more basic extractions. So I mixed in Calcium hydroxide to the cactus powder (same as previousy used) & added more ethanol.
What resulted this time was a lot lighter, see through yellowy ethanol. Its evaporating now but is very different from the 1st pull.

The very different colours could be explained by it being the 2nd pull, or due to the Calcium Hydroxide limiting what's being pulled out by the alcohol. I'm favouring the 2nd option.

At this point I thought I'd try something else for balance so added some hydrochloric acid (and a little water) to the cactus powder. Then added ethanol. This produced a darker greeney very cloudy (though not with sediment/powder as this all settled) ethanol. This was also very difficult to vacuum filter. Any ideas why?
Its evaporating now but is a lot darker than the basified pull and greener. Interestingly it seems to be evaping quicker than the basified pull too - though this may be due to other factors (position, temp, water consistency).

What I'd like to know is this - what difference has the base & acid made to what has been pulled out from the san pedro?
Which is likely to have the most mescaline (leaving aside 1st, 2nd, 3rd pull issues)?
and what else is likely to be present (or won't be present) in each?

If anyone can answer this, and give me some idea of they why behind it I'd be very grateful.

 

[mew]

i doubt your ethanol is 100, so being partly comprised of water and part ethanol id say you got most of the alkaloids in your first pull

by freebase mesc alkaloids are an oil

hcl will convert all salts to hcl, though in your case there were little to none left

 

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Wanted to update on this as I've now evaporated & weighed all 3 pulls - the 2nd basified pull took ages to evap.

Weights and descriptions are as folows:
1) 1st ethanol extraction - 9.281g of very dark brown/black resin. melts easily when left unrefridgerated.
2) 2nd basified extraction- 4.523g of oily yellowy stuff, when scraped comes off evap tray in thin crumbly sheets.
3) 3rd acidified extraction - 8.355g very sticky light browny greeny resin. Was very sticky when scraping off the evap tray. Haven't left unrefridgerated.

Have to say I'm surprised with the weights that're coming out as I'd only started with 62g of dry cactus powder.

If I have pulled most of the mescaline in the 1st pull presumably 3) contains other alkaloids. Any idea if they're likley to be active on their own account, or add to the experience if taken with the 1st batch?

Any idea why there's so much in 3), I'm sure a lot of weight is still ethanol residue as its so sticky but still, I was expecting hardly anything.

If 2) is (in part) mescaline (and other alkaloid) freebase will I be able to smoke this? If so what'd be a necessary dose?

I plan of sampling each of these products when I have time & will post results here.

 

[mew]

your first pull was full spectrum including plant oils and alkaloids

your second pull was contaminated with base

your third pull was the resulting reaction of hcl and naoh giving you nacl, in addition to whatever the acid did the cacti powder (broke it down and made it hard for you to filter) leaving you with a lot of nothing, but with something small in that nothing never the less

perhaps you might take the second and third extraction and wash with acetone ( i understand that both freebase and hcl mescaline are acetone soluable )

 

[benzyme]

a wash is just that... something to wash impurities from your product. it wouldn't make sense to use a solvent you'd discard if your product was soluble in it. mesc salts are not soluble in acetone, which is why it's so easy to freeze precipitate them

 

[mew]

Benzyme Y U NO BE HAPPY?!~?

no i really meant to say selectively dissolve the desired alkaloids while leaving the trash undissolved behind. if in fact mesc salts / freebase are insoluable at the very least then you could "wash" away some impurities with acetone (as long as its dry)

 

[benzyme]

what you'd want to do is rinse the salts with cold isopropanol or acetone, then a cold nonpolar, while applying vacuum. then scrape the cleaned crystals from the filter paper. that's a proper washing.

 

[The Day Tripper]

your third pull was the resulting reaction of hcl and naoh giving you nacl

Since he used caoh, i believe it would be calcium chloride. Its fairly soluble in water, and acetone to an unknown degree. If he used wet ethanol, or did not fully dry after adding caoh then hcl, perhaps that could be the contaminant in the 3rd pull.

As far as where to go from here, i would mix them all together, dissolve what will in warm hcl water, filter and evap. Repeat 3x. (the mescaline hcl will be extremely soluble, fats oils and other crap not so much at all). then take what you scraped up after evaping the hcl water, and basify again with caoh and water, making a paste, then drying fully. Pull 3x with a dry alcohol, or acetone. 95% etoh prob will work, but there will be contaminants from the water being there, no big deal as calcium chloride is food safe at amounts of 400mg daily (what you are already getting in your diet).

Finally add hcl to your acetone/etoh/other alcohol containing freebase mescaline, and evap. Scrape up and store after drying fully. Alternatively if the solvent is absolutely dry, and you want to go to the trouble or can, bubble hcl gas through your dry alcohol to precipitate mescaline hcl crystals.

 

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Thanks for the useful info guys, looks like I might not get much out of sampling the basified & acidified resins after all.

Mew, Benzyme, I'm not sure I follow, will both freebase & salt mescaline be insoluble in anhydrous acetone? I'd always thought both were but you guys know more chemistry than I.

Presume I'd need to do that with the resin as is, that is not dissolved in anything (other than acetone) so would hot acetone work, I'm thinking otherwise the soluble stuff might not all dissolve.

Day Tripper, Likely Calcium Chloride is the contaminant as there was water in the mix.
I'm sure you'r suggestion will work, it just looks like a lot of work, lots of evaping & rehydrating. I'm looking for something quicker given its likely to yield a small quantity of mescaline - I'm keeping the 1st full spectrum pull as it is).

I think I'll go with the acetone idea or just dissolve in hot water, pull with limonene add hcl water to limonene then evap hcl water.

 

[mew]

mesc hcl is insoluble in dry acetone, if your acetone is not dry then you may lose some of your alkaloids to the water solubility

im unsure of fb solubilties

 

[dg]

what you'd want to do is rinse the salts with cold isopropanol or acetone, then a cold nonpolar, while applying vacuum. then scrape the cleaned crystals from the filter paper. that's a proper washing.

yeah, but he's got 20+g of crud from 60g of cacti

i'd throw out the 2 last attempts, and eat the 9g of resin from the first run.

 

[mew]

id eat the 9 g resin after a calorie free day of fasting

the last two id mix with water and let them neutralize each other, bassify. let dry again. powder. cover with nps. pull 3x nps, salt 3x all nps at once. clean salts if your still using hcl

 

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Yeah, I was already planning on eating the 1st pull seperately.

I've combined the other 2 pulls and dissolved in water. I'm evaporating them now. Out of interest what's the benefit in evaporating them & running NPS over powder versus just keeping the alkaloids dissolved in water & mixing in NPS then separating?

 

[Shelzdatripp]

Hi can I ask is it ok to dry fresh cacti in low temp oven or would you suggest dry naturally?

 

[shroombee]

Hi can I ask is it ok to dry fresh cacti in low temp oven or would you suggest dry naturally?

Either will work. The oven will be faster. I use a dehydrator.