We've Moved! Visit our NEW FORUM to join the latest discussions. This is an archive of our previous conversations...

You can find the login page for the old forum here.
CHATPRIVACYDONATELOGINREGISTER
DMT-Nexus
FAQWIKIHEALTH & SAFETYARTATTITUDEACTIVE TOPICS
Piperine extraction ? Options
 
sigmundfreuid
#1 Posted : 7/26/2010 5:53:16 AM
DMT-Nexus member


Posts: 374
Joined: 07-May-2010
Last visit: 15-Oct-2013
Hi, i just saw Phlux's pics from Mycotopia of his Piperine X-tals and i trully was amazed by them. (you have to be registered to see them.)

I would love to know how to extract it just so i could grow some really nice crystals from piperine.

I was wondering where can i find a straight forward tek for the extraction of piperine from pepper for simpletons ?

I do not own any lab ware, i can get 70% to 99% IPA, Acetone,naphta,HEET,i cant get 95% ethyl alcohol, too expensive.etc. + calcium hydroxid,NAOH , KOH ,acetic acid, citric acid .







It would be great if Phlux or Director of Sound had a pictorial of their x-traction .

Thanks in advance.
Swim is a figment of your imagination and he's a compulsive liar,thus everything he says is pure lies !
 

Live plants. Sustainable, ethically sourced, native American owned.
 
Xt
#2 Posted : 7/26/2010 5:46:31 PM

.

Senior Member

Posts: 981
Joined: 24-Dec-2009
Last visit: 13-Oct-2022


Quote:
Extraction process 1: Extraction of Piperine from black pepper
Piperine
Piperine forms monoclinic crystals or prisms when recrystallized from alcohol. The crystals have a melting point of 130 Celsius. The crystals are at first tasteless, but then rapidly impart a burning taste when ingested. Piperine is insoluble in water, slightly soluble in alcohol, and soluble in chloroform, benzene, and acetic acid. Piperine is readily extracted from black pepper, and is one of the chief compounds responsible for the characteristic taste of black pepper.
Method 1: Extraction of piperine from black pepper
Materials:
1. 75 grams (2.6 oz.) of powdered or finely ground black pepper
4. 65 milliliters (2.2 fluid oz.) of warm water
2. 750 milliliters (25.3 fluid oz.) of 95% ethyl alcohol
5. 65 milliliters (2.2 fluid oz.) of more water
3. 50 milliliters (1.7 fluid oz.) of a 10% potassium hydroxide solution in 95% ethyl alcohol
6. 100 milliliters (3.4 fluid oz.) of acetone
Hazards: Wear gloves when handling potassium hydroxide, which is very corrosive. Extinguish all flames before using ethyl alcohol, and acetone, both of which are flammable.
Procedure: Into a standard reflux apparatus, place 75 grams (2.6 oz.) of powdered or finely ground black pepper (if using fresh black pepper corns or granules, the corns or granules should be finely ground before using). Note: 75 grams of black pepper is about 2/3 of a normal bottle sold in the grocery store. After adding the black pepper to the reflux apparatus, add in 750 milliliters (25.3 fluid oz.) of 95% ethyl alcohol. Thereafter, reflux the mixture at 78 Celsius for about 4 or 5 hours. After the reflux extraction process, remove the heat source, and allow the alcohol mixture to cool to room temperature. Thereafter, filter the alcohol extract to remove insoluble materials, and then place this filtered alcohol extract into a distillation apparatus, and distill-off the ethyl alcohol at 78 Celsius until the total remaining volume is about 75 milliliters (2.5 fluid oz.). When most of the ethyl alcohol has been removed, and the left over remaining alcohol concentrate is around 75 milliliters (2.5 fluid oz.) in volume, stop the distillation process, and collect the left over remaining alcohol concentrate (after it has cooled), and place it into a clean beaker. Then, into a second clean beaker, add in 50 milliliters (1.7 fluid oz.) of a 10% potassium hydroxide solution in 95% ethyl alcohol. Thereafter, to the potassium hydroxide/alcohol solution, add in the concentrated alcohol extract, and thereafter, heat the total mixture at about 60 to 70 Celsius. When the temperature of this mixture reaches 60 to 70 Celsius, slowly add drop wise, 65 milliliters (2.2 fluid oz.) of warm water. Note: during the addition of the water, the desired piperine compound will gradually precipitate. When precipitation begins, remove the heat source, and allow the alcohol mixture to cool to room temperature, and during this cooling period continue to add the water, slowly and drop-wise. When the mixture has cooled to room temperature, add in 65 milliliters (2.2 fluid oz.) of more water (cold water this time), and then stir the entire mixture for about 30 minutes at room temperature, and then allow the entire mixture to stand (no stirring) for several hours at room temperature. Afterwards, filter-off the precipitated solid, and then vacuum dry or air-dry it. Finally, recrystallize this dry solid from 100 milliliters (3.4 fluid oz.) of acetone, and after the recrystallization process, vacuum dry or air-dry the filtered-off crystals. The result will be about 3 grams (0.1 oz.) of the desired piperine compound with a melting point of 128 Celsius.
19


Figure 010. Reflux apparatus equipped with drying tube for the extraction of piperine from black pepper. Cold water should be circulated through the reflux condenser jacket.

“Right here and now, one quanta away, there is raging a universe of active intelligence that is transhuman, hyperdimensional, and extremely alien... What is driving religious feeling today is a wish for contact with this other universe.”
― Terence McKenna
 
sigmundfreuid
#3 Posted : 7/26/2010 6:32:39 PM
DMT-Nexus member


Posts: 374
Joined: 07-May-2010
Last visit: 15-Oct-2013
Thanks for the tek , but like i said, i have no labware,i only have the basic things people have .
Swim is a figment of your imagination and he's a compulsive liar,thus everything he says is pure lies !
 
Xt
#4 Posted : 7/26/2010 6:40:57 PM

.

Senior Member

Posts: 981
Joined: 24-Dec-2009
Last visit: 13-Oct-2022
Sorry dude,
Id make up some 10% IPA / KOH, gently heat the solution and add ground pepper, heat for an hour, filter, Add some water to crash out the piperine, filter the solution, collect the filter cake and recrystallize with acetone.

That should do it,
Or you could try this:

Quote:

10kg dried fruits of p nigrum l ... were crushed and extracted 5x with EtOH at room
temp. after removal of solvent in vacuo, the syrupy residue was left overnight at room
temp. when a white crystallizate sept out, which was filtered. on recrystallization from
MeOH it formed 50.54g fine needles, mp 128-129°, and was identified as piperine.


“Right here and now, one quanta away, there is raging a universe of active intelligence that is transhuman, hyperdimensional, and extremely alien... What is driving religious feeling today is a wish for contact with this other universe.”
― Terence McKenna
 
Ginkgo
#5 Posted : 7/26/2010 7:15:25 PM

DMT-Nexus member


Posts: 1926
Joined: 10-May-2009
Last visit: 27-Apr-2015
Location: ☂
Phlux also has a thread about the subject in our forums. He states himself that it was "extracted with ipa - bombed out with water - filtered and re-x'd with ipa". That is incredible easy, and you should be able to do it without any labware.
 
sigmundfreuid
#6 Posted : 7/26/2010 11:28:49 PM
DMT-Nexus member


Posts: 374
Joined: 07-May-2010
Last visit: 15-Oct-2013
i really wish Phlux or Director of Sound would make a tek ,not necessarily with pics ,just something i can easily follow
Swim is a figment of your imagination and he's a compulsive liar,thus everything he says is pure lies !
 
Gir
#7 Posted : 7/26/2010 11:38:26 PM

Gir

Senior Member

Posts: 403
Joined: 17-Jan-2010
Last visit: 18-Jun-2018
Location: on the banks of Shangri-La, and Im nekkid!
sigmundfreuid wrote:
i really wish Phlux or Director of Sound would make a tek ,not necessarily with pics ,just something i can easily follow


Can you not easily follow directions?

1. take pepper and grind them up
2. take ipa and add it to the pepper (EXPERIMENT FOR THE RIGHT AMOUNT)
3. (obviously) stir the solution to saturate it with piperine
4. filter out solids
5. add water, be amazed as you see piperine crash out
6. FILTER SOLUTION
7. collect filtered material
8. heat up some acetone, and add piperine crystals
9. Slowly evaporate for largest crystals.

Next time...

Experiment?
Lets go extract something together Smile

house wrote:
19:10:05 ‹house› mama aya gave me lego man eye healers


Smoke Spice, NOW

Gir likes to tell lies, and the truth, but gir cant even tell the difference between them...


http://www.thevenusproject.com/index.phpTHIS IS THE VENUS PROJECT.
 
Xt
#8 Posted : 7/27/2010 7:27:23 PM

.

Senior Member

Posts: 981
Joined: 24-Dec-2009
Last visit: 13-Oct-2022
There is also this method... just heated with IPA and CaCO3, the carbonate helps keep the extraction clean.
Then some of the IPA is distilled (or evapped) off and so the solution becomes super saturated, it is then cooled and the piperine will precipitate out.

Not sure which one of these methods is best as i have never tried it.

Quote:
isolation of piperine from black pepper

piperine, a very weakly basic substance, can be isolated from a variety of peppers
by extraction with alcohol. ... piperine, along with a small amount of its Z,E isomer,
accounts for about 10% of the weight of black pepper.

procedure
place 15g of ground black pepper and 1g of powdered CaCO3 (1) in a 250mL
boiling flask, add 100mL of IPA, and, after fitting the flask with a reflux condenser,
boil the mixture for about 1h on the steam bath. at the end of the heating period,
filter the mixture by gravity into a 125mL erlenmeyer flask, clean the 250mL
boiling flask, and return the filtrate to the boiling flask. fit the boiling flask with a
distillation adapter and condenser, and boil off all but about 10mL of the IPA (2).
transfer the residual solution from the boiling flask to a 25mL erlenmeyer flask,
and set the flask aside to cool for crystallization of piperine (3,4). collect the product
by suction filtration, using small portions of MeOH to rinse the flask and wash
the product. yield: about 0.5g.

(1) the addition of CaCO3 should prevent the extraction of acidic
components of pepper

(2) IPA boils at 80°C, only a little below the maximum temperature attainable on
the steam bath. to make the distillation proceed quickly, clamp the boiling flask so
that it is well down in the rings of the steam bath, and drape a towel over the flask
and the steam bath to make a tent that will hold steam around the top of the flask.

(3) crystallization occurs slowly, and the flask must be allowed to stand for
at least 24h.

(4) alternatively, add 25mL of water to the IPA solution of piperine, allow the mixture
to stand for at least 24h so that precipitation will be complete, collect the solid by
sucction filtration, and recrystallize it from either IPA or acetone.



PS: Do let us know how it went, or throw up some glittering shiny pictures!

“Right here and now, one quanta away, there is raging a universe of active intelligence that is transhuman, hyperdimensional, and extremely alien... What is driving religious feeling today is a wish for contact with this other universe.”
― Terence McKenna
 
rOm
#9 Posted : 1/16/2011 7:56:16 PM

DMT-Nexus member

Senior Member

Posts: 2096
Joined: 20-Nov-2009
Last visit: 12-Nov-2023
the method work.
Just tried the simplest due to non access to caCO3.
99% IPA pull, water bombing, decanting, vacuum filtration and lil xtals are here. Not a lot though.
No time to re-x with IPA.
Smell like tea n,n spirit !

Toke the toke, and walk the walk !
 
alphacheese
#10 Posted : 7/12/2013 6:10:44 AM
DMT-Nexus member


Posts: 1
Joined: 12-Jul-2013
Last visit: 12-Jul-2013
I've had some success with piperine extraction. I would recommend investing in some minimal lab gear. Ebay is almost exclusively where I get mine. I've accumulated a fairly decent lab over the last few years. Sorry I don't have any pictures and I am still perfecting my process. I have tried refluxing in RBBF and I must say that this is an extraordinary waste of time. Sure it works but you are going to reflux for hours and only yield a few grams of product. I'm very anal about efficiency and thoroughness so I use a soxhlet and run it until the return liquid is completely clear. I run several soxhlet extractions with about 750mL IPA in a 1000mL RBBF and can yield quite a bit of piperine this way in the same liquor.

I found this paper outlining the design of an improvised soxhlet. It still requires some labware. However, with some ingenuity and imagination you could make something of the sort with some rubber stoppers, glass tubing, jars, and a pressure cooker. I haven't yet built a large scale soxhlet but I have constructed a few small scale ones for an algal growth experiment. The idea is quite simple. The return tube functions as a siphon. adjusting its height relative to the soxhlet will determine the amount of liquid that will flow into it before it empties.

My small scale soxhlet uses aquarium tubing because I'm running room temperature water. The outlet tubing from the boiler would need to be high temperature resistant, preferably glass but the return tubing could possible be a temperature tolerant synthetic tubing. Provided it can handle the solvent you are using.

Here's a link to the improvised soxhlet idea. http://www1.datafilehost.com/d/3572ca64
 
 
Users browsing this forum
Guest (2)

DMT-Nexus theme created by The Traveler
This page was generated in 0.027 seconds.