My friend needs some help with his first Mescaline extraction.

So my friend put 100 grams of relatively dry relatively powdered what he thinks is San Pedro cactus (he just powdered 12 inches or so, not specifically the green flesh) in 2 L of distilled Water and 50 g of NaOH. 500 mL of Xylene was added and then shaken. After 24 hours 350 mL of Xylene was pipetted out (it was getting to be a pain to get any more easily) and mixed with 100 mL of water with ~.1 mL of 30% HCl (litmus paper reads ~3.5). This was shaken and after 6 hours stuck in the freezer. After the aqueous phases froze the Xylene was poured back into the jar with the cactus. The water was evaporated and nothing was there.

My friend and I came up with a few possibilities for what happened:
1. Not enough NaOH
2. Not enough HCl
3. Freezing causes the Mescaline to migrate back to the Xylene.
4. The cactus doesn't contain Mescaline. Which would be a gigantic bummer.

Any help or ideas would be great.

EDIT: There is a little something left in the pan. I scraped this very thin layer up and its yellowish brown, no more than 20 mg. I didn't notice it at first because the layer is so thin.

I would think your method worked. You added enough lye and I believe enough hcl acid. You might have the wrong cactus, there are so many lookalikes. Most cactus should produce at least something from this extraction, so that could be 20 mg of natural non-mesc alkaloids.

It's hard to tell. If the cactus was the whole flesh not just the good parts your yield probably wouldn't be over 0.2-0.3% even if it was san pedro. That is 100-150 mg if you got 100% of the alkaloids out of 50g. Usually the first xylene pull gets around 50% I believe, so that is 50-75 mg. You got about 2/3rds of the xylene out so that is down to 33-50 mg. So you might have the real cactus and just didn't use enough cactus.

Not sure if you used enough HCl but I know you used enough lye. I should think .1 ml of 30% is fine, I usually used 3-5 drops (prolly .2 ml) in 100 ml water for 100 grams cactus and didn't even use it all and was successful. So I think your method is sound. Has anyone tried the cactus in a tea or anything to know if 12" is sufficient?

I do a bit larger extractions, and I use more lye than cactus, but the important thing is that you get the pH high enough. If you get the pH of the lye water above 12-13 you should be fine. My guess is that you probably don't have the right cactus, or one that is very potent, if it is the proper species. I had a lot of attempts on fresh cactus fail due to them being weak specimens. Achuma (Trichocereus bridgesii) tends to be the most potent after peyote (Lophophora williamsii), or buying dried cacti chips (Trichocereus pachanoi or peruvianus) or powder from a reliable vendor can help you ensure that you are getting a quality starting material.. The acid water sounds fine, and the mescaline will not go back into the solvent when the water is frozen, unless it is made basic. So, even frozen acidic water will hold the mescaline.

if the basic phase was goopy when the xylene was pulled, this means the cells were not fully lysed. it should have a runny or syrupy consistency.

what may have been leftover after evaporating the water was some cacti cellular membranes and pigment.

I have some more cactus which I can try it on, this time I'll decore and skin it for a higher yield.

I had another thought recently. There is a whitish layer just below the naptha that I assumed was the skin of the Cacti. I pipetted some of this stuff up and its looks like I imagine liquid fat would like. Is there any chance that the mescaline migrated to this instead of naptha?

naphtha? or xylene?

Xylene, sorry about that.