Substance testing Qualitative analysis of citrus reticulata leaves via pyrolytic organoleptic testing

[vlad665]

Cca 50 g fresh citrus reticulata leaves were blended with 250 ml distilled water.
Ph was lowered to 3 using HCl, and blended again.
The mix was defatted with cca 100 ml extraction benzen, followed by separation and a rough filtration using a 0.5 mm sieve mesh
The fraction was alkalinised to ph 14 with NaOH then moved to a flask.
100 ml extraction benzen was aded on top of the mix and it was vigurously shaken.
All solvents were used at room temperature.
The flask was left to settle cca 15 minutes, and the non polar fraction recovered and poured in a pyrex dish, then moved to the freezer set at -20°C.
2 hours later, the pyrex dish was recovered from the freezer, the solvent poured into a beaker, and the water droplets along with some residual precipitation was scraped from the pyrex dish, and the tray was cleaned and dried. The solvent was then poured back into the pyrex dish and set back into the freezer.
The frozen water droplets along with some scrapings were recovered into a stainless steel spoon that was heated with a lighter untill all the water evaporated. The residue in the spoon was slowly vaporised aswel, leaving the unmistackeable burnt indol scent specific to n,n-DMT freebase.

 

[Varallo]

cca 50 g fresh citrus reticulata leaves were blended with 250 ml distilled water.
ph was lowered to 3 using hcl, and blended again.
the mix was defatted with cca 100 ml extraction benzen, followed by separation and a rough filtration using a 0.5 mm sieve mesh
the fraction was alkalinised to ph 14 with naoh then moved to a flask
100 ml extraction benzen was aded on top of the mix and it was vigurously shaken.
all solvents were used at room temperature.
the flask was then left to settle cca 15 minutes, and the non polar fraction recovered and poured in a pyrex dish, then mkved to the freezer set at -20°C.
2 hours later, the pyrex dish was recovered from the freezer, the solvent poured into a beaker, and the water droplets along with some residual precipitation was scraped from the pyrex dish, and the tray was cleaned and dried. the solvent was then poured back into the pyrex dish and set into the freezer.
the frozen water droplets along with the scrapings were recivered into a stainless steel spoon that was heated with a lighter till all the water evaporated. the residuu from the spoon started vaporising aswel, leaving the unmistackeable burned indol scent specific to n,n-DMT.

From experience, I do know that many plant extracts can produce an indole-like smell when they are vaporized or burned. So on its own, that isn’t really conclusive evidence.

That said, you could increase the scale of your extraction and see whether you end up with a quantity that is sufficient to further clean up and crystallize. Or better yet you could use TLC to determine whether it actually contains our favorite compound.

In any case, it’s an interesting experiment.

Note:
I’m assuming, and I do hope, that you are using an untreated orange tree for this, because otherwise there’s a fairly high chance you’d be extracting pesticides that were sprayed onto the leaves.

 

[vlad665]

From experience, I do know that many plant extracts can produce an indole-like smell when they are vaporized or burned. So on its own, that isn’t really conclusive evidence.

That said, you could increase the scale of your extraction and see whether you end up with a quantity that is sufficient to further clean up and crystallize. Or better yet you could use TLC to determine whether it actually contains our favorite compound.

In any case, it’s an interesting experiment.

Note:
I’m assuming, and I do hope, that you are using an untreated orange tree for this, because otherwise there’s a fairly high chance you’d be extracting pesticides that were sprayed onto the leaves.

the leaves were aquired at regular supermarkets. the crates come with a ton of leaves. i just filled 2 bags of leaves, along with 2 fruits in each bag, weighed and payed as mandarines. once home i washed them all with soap and hot water, rinsed then proceded to blend them.
also, after lowering ph, a defat was done, to eliminate any lipophilic compunds, and most systemic pesticides are lipophilic

 

[vlad665]

From experience, I do know that many plant extracts can produce an indole-like smell when they are vaporized or burned. So on its own, that isn’t really conclusive evidence.

That said, you could increase the scale of your extraction and see whether you end up with a quantity that is sufficient to further clean up and crystallize. Or better yet you could use TLC to determine whether it actually contains our favorite compound.

In any case, it’s an interesting experiment.

Note:
I’m assuming, and I do hope, that you are using an untreated orange tree for this, because otherwise there’s a fairly high chance you’d be extracting pesticides that were sprayed onto the leaves.

anyway, the fraction of extraction benzen recovered after 1st freeze where i discarded the frozen droplets, was put back in the freezer. 2 hours later this is whats in the dish. the solvent still milks out when i blow on it, so i suppose theres still enough to crash. will check again later in the evening, maybe i can fix a pc cooler to evap some of the solvent and suprasaturate it

 

[Varallo]

the leaves were aquired at regular supermarkets. the crates come with a ton of leaves. i just filled 2 bags of leaves, along with 2 fruits in each bag, weighed and payed as mandarines. once home i washed them all with soap and hot water, rinsed then proceded to blend them.

Ai okay, be extra careful and don’t bio-assay without knowing if you’re leaves are clean from pesticides.

 

[vlad665]

Ai okay, be extra careful and don’t bio-assay without knowing if you’re leaves are clean from pesticides.

they should be clean for the most part, due to soap wash and defat. i dont panic at trace ammounts, anyway, and the bioassay is mandatory to deteeminte wtf i had pulled from those leaves