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Rue Extraction: base precipitation incomplete!? Options
 
Juremo
#1 Posted : 8/23/2012 12:01:37 PM
Hello,

Doing a Syrian Rue alkaloid extraction for the first time, I am a bit insecure how to proceed... or if I messed something up.
I would greatly appreciate, if someone with experience can help me out.

Let me summarize what I did up to now:

1. I extracted 100g of (coarsely ground) Syrian Rue seeds 3 times with ~1l water (acidified with acetic acid).

2. I filtered twice, the second time through a coffee filter.

3. I boiled it down to around 200ml (forgot it on the stove to be honest)

4. i diluted it with dH2O to 500ml and added around Sodium Carbonate until the dark brown color had changed to a coffee-with-milk color, adding more does not change the color anymore (used around 3 teaspoons).

5. I put it in the fridge in a 500ml Erlenmeyer, after 8 hours, there is only a 1cm layer of light-brown suspension on the bottom. The rest of the liquid is still opaque dark brown. Carefully swirling around the liquid covers the flask's neck with a thin bright yellow layer.

I don't really want to decant now because it would leave me with around 100ml and I suspect a lot of alkaloids are still in there. The two "layers" have only a very slight color difference.
The solution seems saturated now if I add more soda it forms clumps on the ground.

Should I add more water and then more soda (or NaOH)?
Or is is just a low yield and I should continue as usual?

Regards,
and thanks in advance for a quick answer Smile
 
3rdI
#2 Posted : 8/23/2012 12:07:43 PM
i would bang some lye in there and see what happens
INHALE, SURVIVE, ADAPT

it's all in your mind, but what's your mind???

fool of the year

 
Juremo
#3 Posted : 8/23/2012 5:06:40 PM
Quote:
i would bang some lye in there and see what happens


I took 20ml of the brew and added diluted lye to it in a test tube.
after nothing happened i even threw some NaOH pellets in (frustrated...but carefully)

no color change...not even around the pellets

alkaloid-less rue? did I destroy the alkaloids by boiling it down too long?

Any more ideas? please?

I wish I had kept some of the seeds to eat them as is...
 
 
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