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Harmala alkaloid extraction ( Passiflora Caerulea ) pictorial ! Options
 
Ambivalent
#1 Posted : 12/31/2011 8:22:06 PM

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As i mentioned, i prepared a pictorial on how the extraction process went ( i was in a bit of rush aand it is my first, so the pictorial is not of the best quality ) :

I found that if you are working with basic kitchen equipment and not more advanced and more suitable equipment for your method of extracting, the patience is always THE key to successful and clean extraction.

Plant Material : 200-300 g fresh plant material of Blue Passiflora (my first assumption was that i used around 400-500 g fresh plant material, but when we actually measured what we visualy thought is 500g, was more close to 300 g.
EDIT : The plant i harvested grows in the southern Balkan. The climate here usually varies, the summer's are hot and the winter's moderately cold.Last two winters are pretty warm. We had temperatures above zero more than half december, and now january also.Bottom line is, I don't know how variable are these species..especially when they are adapted on a climate which is not native to them. This is something that i will also try to document and confirm.

Acid : Acetic and Phosphoric

Base : NaOH, baking soda

Measurements were made with really accurate PH meter which also compensates on temperature changes.
(I think for these kind of extractions, a good PH meter is a must if you want clean and successful extraction.) Thats why i usually don't measure volumes of how much acid or base i'm adding.


First i let the plant material to soak in cold water for at least 30 mins, or hour. My goal was to wash of any contaminants that might be on the leaves and other parts of the plant, because it grows in an urban area where a lot of vehicles pass by every hour.


After that i covered the plant material in water and i acidified with Acetic acid (used around 30 or 40 ml) till the PH meter readed 3.50 , 3.60

The cooking plate was set to slowly cook the plant more like brewing a tea, not really boiling temperature.
After few hours of brewing and occasional mixing i filtered and got around 2 and a half liters of orange liquid.


only a small amount of the brewed tea

The tea was left on cold temperature overnight and the next day was filtered once more from the plant material that has accumulated on the bottom.It was than reduced first on half the volume, than filtered again to keep it as clean as it can be before basing. Than reduced again at approximately half liter and of course filtered once more.

At the first basing i was using NaOH for base which i powdered before i added it.I was adding veery small amount's and was mixing slowly to help it dissolve quicker.Total base added was almost equivalent on the acid used in the first acidification, around 3 g . After each few pinches of base added, the Ph was tested.The precipitation was visible around Ph 7 . I based until Ph 9 . This is the jar after the basification, but the precipitates are almost all collected, only small amount can be seen on the very bottom.

the jar with the tea after the basification

From here i very simply followed Gibran's TEK for further cleaning and extracting the freebase alks.
This next photo is after one or two washes of the precipitates with slightly basic water.



another photo of washing the precipitates (the color of the water looks cleaner here) , but the precipitates still have darker color !




After i cleaned the basic water sufficiently i decanted the water and i made acidic solution with Phosphoric acid.I then dissolved the precipitates and left them over night ( this step required some more time and patience ) .
The next day there was some insoluble impurities on the bottom just like on Gibran's Tek . The solution was decanted and then again based with baking soda adding only enough to precipitate the alkaloids. Carefull measurement is needed not to over do it, less cleaning steps are needed later if done properly.


the precipitates washed with slightly basic water


second wash of the precipitates

The third and fourth washes were done with normal tap water.The water in my city is pretty basic ( slightly above Ph 7 ) so i think its ok.




The water was then decanted as much as possible.The work was done with help of plastic syringe.The drying is the part i find most time consuming. I was drying with moderately hot air but was afraid not to over do with heat.





This was the final yield which on my scale showed 940 mg . It should be relatively pure, because it gets completely diluted in acidic water with no or very little residue ( maybe dust or sodium carbonate particles but negligible ).



Thanks to everyone for sharing their resources and experiences, gained by dedication in exploration.

The plant's and the knowledge we gain about our self and others through the experiences they make available for us...These things amongst other's are the most essential occurrences on this planet in all ages of mankind.

All the best in the New Year to everyone, Much Love !!

 

Live plants. Sustainable, ethically sourced, native American owned.
 
jamie
#2 Posted : 12/31/2011 9:06:21 PM

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good work! I would love to see analysis on this stuff though to verify what it actaully is. HCL conversion would be cool to see as well to see if it would crystalize as a salt. Harmine and harmaline hcl is a greenish brown color, while freebase is off white greysih so if it ends up yellowish brown/green as HCL it is most likely harmalas.
Long live the unwoke.
 
smokerx
#3 Posted : 1/1/2012 4:02:21 PM

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great work, thanks for that.
We are each of us angels with only one wing, and we can only fly by embracing one another.

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Ambivalent
#4 Posted : 1/1/2012 9:47:50 PM

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Thanks, i couldn't have done it without you guys at the Nexus !


jamie wrote:
good work! I would love to see analysis on this stuff though to verify what it actaully is. HCL conversion would be cool to see as well to see if it would crystalize as a salt. Harmine and harmaline hcl is a greenish brown color, while freebase is off white greysih so if it ends up yellowish brown/green as HCL it is most likely harmalas.


I would also love to confirm my doubts about what exactly i am playing here with. I mean, how possible is it to be something else besides beta carbolines ?! What else could precipitate out ?


I did some testing with citric acid on this substance in the meantime. 300 mg were dissolved very fast with only couple of lemon drops, and after evaporation there was yellow-green layer that was crystal like ( hard - crunchy ) . Will bio - essay this in small amount's and i will post my finding's
 
jamie
#5 Posted : 4/10/2012 4:29:23 PM

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any updates on the bioassay?
Long live the unwoke.
 
Ambivalent
#6 Posted : 4/10/2012 6:36:32 PM

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Yea, did tested it...

But in any case a real enlightenment was the Passion Flower thread that nen888 opened (thanks nen88Cool..

I understood in that topic that in order to get the full potency of the plant, full spectrum tincture or extract should be made, including the active flavonoids.

My extract was probably mostly harmine or only harmine isolated via the method Gibran2 explained.

- The smoked freebase of the extract prolonged the experience of small ammounts smoked spice ( swim tried 15 mg spice, 60 mg extract ; 25 mg spice, 80 mg extract ; 30 mg spice, 150 mg extract ) The effects of the freebase within the range of 150 mg was subtle and not very strong on its own, a mild antidepressant feeling.

- I also converted some freebase with citric acid,(squeezed lemon juice and filtered)...After evaporation the substance crystallized and it looked quite interesting but during evaporation i contaminated the vessel so i did not bio assayed that batch.
Some time later i converted more of the freebase i had left, only this time i used pure citric acid.So after evaporating i was left with white powder.(i guess the crystallization from the lemon was due to the sugars contained in the juice and not the structure of the citrates)

I bio assayed this powder orally but it didnt activated 50 mg of spice. One thing is that i maybe miscalculated the dose of the extract made with citric acid. Once it was converted with citric acid it gained in mass. I got maybe two times as much salts of this extract than the freebase. So i think i may have miscalculated the right dosage with the citrates and missfired.

After that the winter pretty much skinned the whole plant. Few months after those reports there wasnt even one green leaf on the whole vine. It was a sad sight. I was eager to try making some tincture and orally activating the spice.The only thing that i was worried with tincture of fresh Passiflora Caerulea is the cyanogenic glicosyde which is mentioned on erowid and wikipedia.



 
 
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