Pure piperine xtals (pics)

[DiMiTriX]

yeah it tsartrazine and obviously didn't bought it. i don't remember witch adulterants are in my alchol anyway i'm planning to recryst it wit more alchool food grade an daybe some acetone too.. i red it's good a mix of acetone exane 2/3 or maybe 3/2 i don't remember right now..anyway i'm looking for a nice curcumin extraction now

 

[DiMiTriX]

yeah it tsartrazine and obviously didn't bought it. i don't remember witch adulterants are in my alchol anyway i'm planning to recryst it wit more alchool food grade an daybe some acetone too.. i red it's good a mix of acetone exane 2/3 or maybe 3/2 i don't remember right now..anyway i'm looking for a nice curcumin extraction now

piperine is supposed to be blue fluorescent and it seems to swim,but under his wood black light it doesn't is it fluorescent at 365nm?whitch lenght is wood light?

 

[Crystalito]

Wood's lamp is at 365 nm indeed. I dont know if piperine "glows" under Wood's lamp, but read further: Sometimes fluoresence can be "covered" by heavy color. Other times there is a phenomenon going on called quenching: while one would expect fluorescence to be relative to the concentration of a compound, sometimes you might notice that when you increase the concentration fluorescence goes down because the light emmited gets absorbed by other molecules of the compound (oversimplified explanation). This for example could be the case with harmala betacarbolines where if you go diluting a "non fluorescent under normal fluorescent lamp light" concentrated sample, you will notice that at a point the resulting very dilute sample starts glowing! In this case its a rather nice blue color!

So an idea to try : get a drop of your solution and dilute it under blacklight in a rather bigger volume of alcohol and notice if anything happens!

Speaking of lights, you might be interested also in the ability of piperine to isomerise under light : i do not know the activity of the resulting compounds so try to keep it off light. Check this link : http://www.jstage.jst.go.jp/article/fsti9596t9798/2/1/2_24/_article . Isomerisation products can be chavicine, isochavicine, isopiperine and otheres.

Have a look also at the rather good study i attach. As always , anyone knowing better feel free to correct me.

 

[DiMiTriX]

ok thanks,anway yesterday i put a small ammount of alcohol piperine in water ratio about 1/5 and the liquid turned cloudy....i put all in the fridge and left it set overnight,today not crystals forming nor precipitation on the bottom,always a colloidal solution of piperine that doesn't agglomerate,why? it's EtOH solution

what about put small ammount of water,maybe same quantity of the solution into and let it precip? i saw when you put enbough water that it sink in the bottom in a very cloudy layer that's alomost 'sature' of piperine,maybe swim could left it as it is in the fridge and wait that piperine fall down? i really dunno men,after a night the solution is still cloudy and colloidal,not precipitation at bottom,wha't happen if i boil it a bit? piperine gunk?

 

[Crystalito]

You could give it a go heating it...Consider what you are seeing an emulsion like the one you see when you add water to Ouzo

 

[DiMiTriX]

yup it'ds like ouzo like ,suspension-colloidal thing
swim tried another tek that seems working better..swim concentrated a lot the alcohol solution,put in freezer and separate by the resin gunk at the bottom,than add some vinegar and basified again with naoh solution..there's a nice beige precipitate now on the bottom 8) by now it's powder but maybe it will crystallize or swin just needs to recrystallize it

 

[DiMiTriX]

ok it could seems odd to swim but afoaf has added naoh solution to etanol and water solution of piperine,,it becomes cloudy,than acidified with vinegar still it change slightly bit color again and become strangely a bit clouder...and than rebasify,it turn trasparent and after less of an hour there are crystals at the bottom!! 8) very pure prudught slighly yellowish

 

[DiMiTriX]

theese crystals are very pure and are big as nacl fine powder,swim would recystallize em just to obtain bigger crystals the possibilities are 3: etanol (food safe),acetone paint solvent (surely less food safe) but better as recyst solvent and third a mix of 2 parts of acetone and third of 95% esane + 3% of dichloroethane (swim hasn't pure etane so would use this stain remoover)

the third solvent seems to be the best but the last food safer so swim would recryst in etanol? or etanol and water?or etanol and acetone mix? suggestions nexians please..


swim would try this same procediment of extraction and precipitation from etanol with 20g of mhrb and see what comes out

 

[Crystalito]

Care to explain the reasoning behind ech step? For example what is the vinegar supposed to do?

 

[DiMiTriX]

it is supposed to make piperine acetate,but i founfd it unnecessary,you could use direcly naoh to precipitate it out

 

[Crystalito]

Truth is i have never heard of a piperine salt so i do not know if making piperine acetate is feasible. Is there a refference or an extraction protocol you followed? If piperine were to be extracted as a salt (watersoluble) then this would simplify the procedure given that other compounds of pepper oleoresin would not dissolve in water. I never saw such a method before though , and those who extract peperine with water use hydrotropes and not an acid so i am a bit dumbfounded why people do not use it more if it works (the acid that is.)...

 

[DiMiTriX]

oh sorry i assumed that al alcaloinds for its nature (anfiprotic?) could be salified mm just think to some examples:cocaine hcl,morphine hcl,mescaline sulphate,dmt acetate,quinine hcl,stricnine hcl and much others

 

[justine]

According to wikipedia :

It yields salts only with strong acids.

.

 

[Crystalito]

So Dimitrix, any news on the piperine project?

 

[DiMiTriX]

swim yielded a dirty piperine and a very low quantity..aniway he will try with curcuma when he will buy some of it,curcumine is unavailable here unfortunatly :?