BeeLoyal (Stranger)
08-17-02 01:20
No 346084
      Safrole and Dillapiole from Piper guineense  Bookmark   

I have read these two posts about Piper guineense

324777 , 320161

and to my fortune I found many trees of the Piper species in my back yard.

my question is how to separate the 48% Dillapiole from the leaf oil? 

and how to extract the 4.8 percent Safrole from the Fruit oil?

is vacum fractioning distilation going to be the right course?

I also have a problem with the concept of these specific steam distilations , after I steam distill the fruits what should I do with the distilate? what should come out the other side? is it water and oil ? if do how do I obtain the 0.35% essential oil from that? should I just distill the water off and get essential oil? or is it somthing else that comes the other side?        and regarding the leafs what should I do with the distilate that they give? is it water mixed with the essential oil ?

and again I wonder to myself how I should manage to seperate all the constituents to get Dillapiole and Safrole (from the leaf or fruit respectivly)    ,   I also wonder what are the other 56 constituents in the fruit oil desribed and how they would effect the seperation of Safrole.

please help a working bee :) I promise documented results to come back your way later.

Beeloyal

The war isnt over!
 
 
 
 
    Bubbleplate
(Hive Bee)
08-17-02 22:18
No 346274
      Steam Distillation  Bookmark   

is definitely the method to use. That being said, you can take one of two routes:
1) Apiol, Safrole etc. are very soluable in alcohol. You could take the plant material, leaves, berries, etc. and soak in say 97% Isopropyl Alcohol for a few days, strain, then evaporate as much as the alcohol as possible. Take the remaining liquid, and then steam distill that in a relatively small glass setup. The steam distillation will carry the pure essential oils over and in the receiver you'll have a layer of water, and one or more layers of oil. The oil layers will be on top of the H2O or, as in the case of Safrole bearing oil, on the bottom, depending upon the density of the oil. Then seperate the layers in a Sep. funnel.  You can further refine the oils gathered by fractional vacuum disttillation. I've used this method to produce almost pure Safrole from Sassafras root bark.
2) You could directly steam distill the plant material. This depends upon what type of steam distillation apparatus you're able to procure or build, and the size of it. Obviously when you have plant material that is relatively low in percentage of oil or compound you desire, the BIGGER the better. You could place the leaves in a drum fitted with a condenser and then feed steam from say, a Pressure cooker, into it. You can also do it in glassware on a smaller scale. I've found that a "vertical" style of still works very well; i.e. where steam is fed from bottom flask into an upper flask of material (check out: http://www.heartmagic.com/EOflyerNEW72dpi.jpg for a pic of what I mean) and thence into condenser, etc. Again, you will end up with layer(s) of oil(s) and H2O.
This method produces very high quality of oils and material directly, but on a smaller scale.
The nice thing about Steam Distillation this way is that ONLY volatile organic compounds like Safole, oils, etc. that are immiscible (insoluable) with water will go up and into the steam and be distilled. Any water soluable constituents will mix with the H2O in the biomass flask and then drain back into the steam generator (water) flask. Oils obtained with this method can also be further refined by Fractional/Vacuum Distillation with a Vigreux or packed column.


If they drive God from the earth, we shall shelter Him underground - Dostoevsky