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Mescaline extraction and cactus yields.... Options
 
Infundibulum
#1 Posted : 4/7/2012 12:29:53 AM

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...so how sure are you that the mescaline you have is mescaline (to an acceptable at least 70-80%)? In the absence of analytical equipment, well you really got not much clue. And your yield was REALLY good but for some reason you need 500-800mg for a proper mescaline trip because as it apparently turns out you're a mescaline hardhead or you happen to suspect tolerance from previous week's trip etc?

Well, time to reconsider. After a friend of mine who was extracting mescaline reported back a really generous yield, I got suspicious - especially when he said that his cactus prep kept on yielding more, a little bit at a time, but significantly. He did A/B, boiled down to a small amount of liquid, basified with NaOH, pulls with limonene and salted with sulphuric acid. When I went over to visit him, he showed me his final evaporate proudly - yes, salting the 10th or more pull was still yielding stuff.

I tried it and it barely tasted bitter; on the contrary, it was far more on the salty side, a good indication of sodium - he was practically making sodium sulfate, basically the result of salting of any residual NaOH in the limonene with sulfuric acid... After trying the rest of his batch (after it had been cleaned with acetone washes), it became apparent that it tastes not only bitter (an indication of alkaloids) but also salty, i.e. it was tainted with sodium sulfate.

We took some methanol and recrystallised his product to the point where methanol could not pull anything from his product - mescaline sulfate is soluble in methanol (as well as ethanol) but sodium sulfate is not). Long story short, his generous yield shrieked to 1/3 of his original size, was not salty and of course represented a more realistic mescaline yield. But since mescaline extraction is prone to salt contamination, which is an issue that I've never seen been addressed before, people need to question their cactus extracts and/or take appropriate measures to clean them should any salt byproduct is suspected. I believe that the biggest culprit is the pulls; clear, transparent pulls will minimize and/or eliminate any salt formation, but even slightly cloudy pulls will result in the reaction of the base used for basification (which will be suspended in the NP pull) and the acid used for salting to form the respective salt and taint the yield.

Any questions, ideas, experiences etc are, as usual more that welcome!








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mew
#2 Posted : 4/7/2012 2:03:16 AM

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i think this thread should be called cactus extraction and mescaline yields Smile)
 
Infundibulum
#3 Posted : 4/7/2012 8:46:29 AM

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mew wrote:
i think this thread should be called cactus extraction and mescaline yields Smile)

True that! But I think I'll just leave this mistake as is, as it sounds funny.




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AlbertKLloyd
#4 Posted : 4/8/2012 1:39:16 AM

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limonene and veggie oil seem to be able to grab salts of sodium and calcium which can be an issue, however the structure of mescaline crystals should not be easily mistaken for sodium salts... mescaline salts should be rectangular plates or needles and have a very neat appearance.
 
biopsylo
#5 Posted : 4/10/2012 1:53:22 AM

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thanks for the insights. when you say the yield will be tainted when
acidifying the np.pull, is it possible that yield will be lost, as well? i tried a drytek using caoh. the paste was dried completely, and crushed, pulled with limonene. pulls were cloudy, i know now that it was suspended caoh. when i added fasipa lots fell out, but it was not bitter at all. i never got any yield.
if limonene is cloudy, let it sit, and it will clear up.
 
AlbertKLloyd
#6 Posted : 4/10/2012 9:10:40 PM

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biopsylo wrote:
thanks for the insights. when you say the yield will be tainted when
acidifying the np.pull, is it possible that yield will be lost, as well? i tried a drytek using caoh. the paste was dried completely, and crushed, pulled with limonene. pulls were cloudy, i know now that it was suspended caoh. when i added fasipa lots fell out, but it was not bitter at all. i never got any yield.
if limonene is cloudy, let it sit, and it will clear up.


I think letting it dry all the way out was the problem, that never worked for me.
I experimented with dry-tek methods for years before abandoning them in favor of STB, the drier the method the less effective it was for me, it didn't work at all for me when I dried the material totally, maybe I did something wrong, but when it was wetter it worked better to a degree, though i always got my best results from totally wet/soup like extraction methods
 
Infundibulum
#7 Posted : 4/10/2012 9:58:11 PM

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AlbertKLloyd wrote:
limonene and veggie oil seem to be able to grab salts of sodium and calcium which can be an issue, however the structure of mescaline crystals should not be easily mistaken for sodium salts... mescaline salts should be rectangular plates or needles and have a very neat appearance.

Yes, crystal shape is a good indicator, but mescaline crystals do not always come out as nice and perfect, especially if one is quickly evapping the acid pulls in an oven. In the latter scenario mescaline and other cactus alkaloids tend to be more amorphous and similar-looking to other contaminating salts. Mesc crystals do come out spectacular after re-x in a methanol or as I remember with the acetone bombing (as reported by Phlux!)

The bottom of the line is that if your NP pulls are cloudy (I suspect that most people's mesc NP pulls are awfully cloudy) then you got great chances of contaminating your alkaloids with unwanted salts...Unfortunately np pulls take a good time (3-4 days) to clear completely. This is a very serious issue when anyone reports mescaline yields. mescaline dosages and most importantly advices on mescaline doses.


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landfishd
#8 Posted : 4/10/2012 11:46:03 PM

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If one titrates carefully when pulling with the acid does this minimize the issue?
 
Spacehippie
#9 Posted : 4/11/2012 2:38:38 AM

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So if one had mescaline hcl. that they suspected was contaminated with salts.What would the cleanup process for it be?
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SnozzleBerry
#10 Posted : 4/11/2012 1:57:56 PM

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Wash with cold, anhydrous acetone, decant the acetone (the mescaline is insoluble), and dry/save the mescaline.

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Spacehippie
#11 Posted : 4/11/2012 2:22:03 PM

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Yes I have already done that.Just didn't know if it got all of the unwanted salts out.Thanks for the info though.
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Infundibulum
#12 Posted : 4/11/2012 6:15:28 PM

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Acetone won't do the trick - One needs something that dissolves mescaline salts but not other salts (that can be sodium chloride, calcium chloride, sodium acetate, calcium acetate and so on, depending on the base and acid used in the process).

The best place to start is by tasting the mescaline; if it tastes bitter and only bitter, then that's good. If it tastes salty, then there are sodium salts contaminating. The taste test won't work if calcium hydroxide was used as a base, as it won't taste of anything.

for cleaning, one can wash the mescaline using methanol and KEEP the methanol discarding what does not dissolve. That is, soak the mescaline in methanol, let stuff settle, then decant and evaporate methanol to get contamination-free mescaline. Do this until evaporated methanol yields no more. Ethanol should also work but mescaline salts are less soluble in ethanol so more will be needed.

Another way is to do a mini-A/B on the mescaline salts to clear them up, this time taking care that the NP solvent is clear!



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SnozzleBerry
#13 Posted : 4/11/2012 6:37:53 PM

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Whoops...please excuse me while I put my foot in my mouth Laughing

So, I assume that one would do the methanol/ethanol cleanup after a mek/acetone cleanup on the cactus extract?
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Infundibulum
#14 Posted : 4/11/2012 7:56:10 PM

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SnozzleBerry wrote:
Whoops...please excuse me while I put my foot in my mouth Laughing

So, I assume that one would do the methanol/ethanol cleanup after a mek/acetone cleanup on the cactus extract?

Yes, but as said above KEEP and evaporate the methanol/ethanol - this is where the goodies areVery happy


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Spacehippie
#15 Posted : 4/11/2012 8:04:40 PM

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Thanks for info Infundibulum.That's what I was looking for.
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landfishd
#16 Posted : 4/11/2012 9:19:34 PM

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landfishd wrote:
If one titrates carefully when pulling with the acid does this minimize the issue?


no? yes?
 
Infundibulum
#17 Posted : 4/11/2012 10:08:30 PM

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landfishd wrote:
landfishd wrote:
If one titrates carefully when pulling with the acid does this minimize the issue?


no? yes?

No, since the issue is with any suspended base/water droplets in the NP solvent that also get salted, not with excess acid. Acid will salt both the mescaline freebase in the NP solvent along with any suspended base non-selectively.

A "careful titration" (I don't know how one would do that!) would serve to minimise the acid contamination and that is only a must to those who salt with non-volatile acids, like citric acid. Excess of volatile acids (like hydrochloric acid and vinegar) as a result of a not so careful titration can be driven away during mescaline drying in, say the oven.


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
landfishd
#18 Posted : 4/11/2012 10:25:07 PM

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OK thanks for clearing that up for me. Forgive me I misread what you initially pointed out and I thought you meant to watch out for a cloudy acid pull which it's been a while I can't remember if my acid pulls were cloudy or not but I think they were and I thought that was a good thing.

So all you have to do to avoid this salt contamination is not get any base water in your NP solvent. I thought this was already a given and fairly simply to do especially if you have a sep funnel and you are not to hasty with the separation.

By careful titration I just meant to leave it under PH7 and being careful not to go over but I guess that is just regular titration technique. As far as I know sulfuric acid is one of those acids that won't dry out right? It is the acid I like to use as it seems to be the easiest to clean.
 
Infundibulum
#19 Posted : 4/11/2012 10:29:25 PM

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yes,

but if the NP solvent pull is cloudy then there will be basic water. only waiting till the np gets transparent guarantees no salt contamination!

Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
jdf121
#20 Posted : 5/16/2012 10:32:29 PM

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So is the NP cloudyness you guys are speaking of before, after, or during salting? My NP is clear when put in the sep funnel, but becomes cloudy when the dilute HCL is added and mixed. The NP stays cloudy until it is put into jars and sits for a few days. Is this indicative of Calcium Chloride formation? Or does NP cloudyness only matter if it is before salting? (Ie. is the NP suppose to be cloudy before the salting?)
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