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first time Phalaris extraction Options
 
John.Brown
#1 Posted : 10/30/2021 5:42:37 PM
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i am in the process of doing an extraction on some wild phalaris arundinacea with some of my aq1 trimmings mixed in. started with ~300g of fresh wet plant material picked at dawn, froze and thawed it several times to ease blending. blended the material, dropped ph to 5 and simmered in closed pan for ~8 hrs. strained through cheese cloth then filtered through coffee filters.

i ran in 2 batches, i simmered the second one for the full 8 while the first one went for only like 4 hrs. the second batch is filtering right now, taking for ever and the filtrate is much darker than the first batch. I am unsure whether this is due to more alkaloids and fats present from the longer simmer or from the filters breaking down. i put some naptha in there to defat the drops as they enter. the filtering has run over 48 hrs know across three different filters.

i have a vacuum filter setup on the way but it wont be here till early December courtesy of the shipping container issues.

when defatting the first batch the naptha remained clear, i do not know if this is normal. i then basified the and added naptha to begin the extraction. once again the solvent remained clear. yellow debris precipitated out of solution and some floats to the top and some to the bottom of the aqueous layer. these could be hydrolyzed fatty acids or some other contaminant.

I will do one extraction of the first batch every week for the next 3, according to the tek im following. i plan to evaporate the solvent and recrys the product in heptane.

attached are pictures of the soutions, the carboy/growler is the second batch currently filtering the Erlenmeyer is the first batch.
any recommendations or notes are welcome.
John.Brown attached the following image(s):
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John.Brown
#2 Posted : 10/30/2021 5:45:38 PM
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Any notes or recommendations are more than welcome.
 
Sidisheikh.mehriz
#3 Posted : 10/30/2021 7:03:42 PM

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Hi there John

I think 8 and 4 hours are not needed waste of energy. Even half to one hour for each cooking is enough. There was no need for filtering either. My teas are never that thick as to not go through a coffee filter easily. Sedimentation during cooking is to be expected and is normal.

Reduce the tea to a smaller volume for a more efficient extraction. Use new fresh growth tips instead of whole leaves. It's much less fats and much more concentrated in the alkaloids you want. There was no need to waste some AQ1 into wild arudinacea. Cook the AQ1 separately when you have enough mass from it.

Use dichloromethane instead of naptha for the initial extraction it's more efficient at extracting than naptha. This is especially more important for such a low yielding plant source like arudinacea. When finished extracting with dichloromethane you can then do a mini acid base extraction using naptha which is very easy.

300g fresh wild arudinacea is barely enough For an extraction so don't expect much from this experiment. Nevertheless it's still a good practice to improve your extraction skills.
 
John.Brown
#4 Posted : 10/30/2021 7:25:49 PM
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Sidisheikh.mehriz wrote:
Hi there John

I think 8 and 4 hours are not needed waste of energy. Even half to one hour for each cooking is enough. There was no need for filtering either. My teas are never that thick as to not go through a coffee filter easily. Sedimentation during cooking is to be expected and is normal.

Reduce the tea to a smaller volume for a more efficient extraction. Use new fresh growth tips instead of whole leaves. It's much less fats and much more concentrated in the alkaloids you want. There was no need to waste some AQ1 into wild arudinacea. Cook the AQ1 separately when you have enough mass from it.

Use dichloromethane instead of naptha for the initial extraction it's more efficient at extracting than naptha. This is especially more important for such a low yielding plant source like arudinacea. When finished extracting with dichloromethane you can then do a mini acid base extraction using naptha which is very easy.

300g fresh wild arudinacea is barely enough For an extraction so don't expect much from this experiment. Nevertheless it's still a good practice to improve your extraction skills.


a few questions, first where do you get dcm/what do you extract it from?
secondly how much mass do you recommend for arudinacea and how much for aq1?
thank you for the info!
 
Sidisheikh.mehriz
#5 Posted : 10/31/2021 8:24:44 PM

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Dichloromethane is sold for 3D printing hobbiests. Or you can distill paint remover that are based on dichloromethane formula. No need for buying a distiller just use the original container as the distiller body and hook a steel or copper tube to the cap and immerse the container Inna warm water bath at 40 celcius. The end of the tube should be immersed in a container filler with chilled water. Add ice as needed to maintain the cold temperatures. The dichloromethane vapor will condense and turn into liquid pouring and drip down to the bottom of the cold jar.
Once finished wash the dichloromethane with brine solution to remove water from the dichloromethane. When distilling near the end try to elevate the temperature a bit so you can distill some toluene that's in the paint stripper formula. It will make the dichloromethane less polar and makes it less likely to form emulations when extracting. Or just add some naphtha to the dichloromethane that will also do.

For AQ1 200g to 300g. For wild arudinacea at least one kilogramme to make something like 40/50mg
 
John.Brown
#6 Posted : 11/1/2021 2:33:59 PM
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Ok, i have a distillation setup (glassware) so that should be no problem. i just moved my aq1 to a bigger windowsill style tub so it should propogate and get me more, also ive fertilized the wild phalaris with ammonium sulfate which should help my next extraction.

In other news, tbere is quite a lot of whitish precipitate from the basification. It looks like it could be fats, noy sure, its kind of stringy. Should k filter the basified mixture?
 
John.Brown
#7 Posted : 11/5/2021 2:37:51 PM
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It seems there is a brownish foam in my naptha layer, should i filter out the naptha?
 
downwardsfromzero
#8 Posted : 11/5/2021 7:06:53 PM

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John.Brown wrote:
It seems there is a brownish foam in my naptha layer, should i filter out the naptha?

You could do, or you could try washing the naphtha with a bit of concentrated brine.




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John.Brown
#9 Posted : 11/10/2021 3:27:24 PM
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i will try that, thanks!
 
 
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