jeffmills
04-02-04 07:13 |
(Rated as: UTFSE!) |
|||||||
Newton (Hive Bee) 04-02-04 20:39 No 498789 |
Better try that on a small scale first... | |||||||
The oil is not volatile so boiling should not be a problem How did you come to this assumption? The 'oil', more precisely the freebase ephedrine, is quite volatile, even at room temperature. Look it up in the Merck Index. For the boiling part... It _does_ evaporate with water vapour easily, that's how steam distillation of Ephedra works. And that's why people acidify the solution, turning the freebase into the HCl salt, before evapping the water off. Note: This is intended for large scale extraction and may be no use for small quantities Better try to get some experience on a small scale first, before dreaming of large scale production. |
||||||||
morpheus (Hive Addict) 04-03-04 03:42 No 498834 |
My general thoughts | |||||||
I have 10 min. before I leave for work so here goes.Have read absolutely nothing on extracting E from Ma Huang or the efedra plant so this is my opinion and maybe wrong. But I think a couple of acid base reductions are required using a base not as strong as NaOH.This is done after removing plant material as you stated with solvents. Gotta go. |
||||||||
jeffmills (Stranger) 04-03-04 06:30 No 498851 |
Ephedrine freebase is volatile | |||||||
Ephedrine freebase is volatile, I was clear on that. But is there any freebase in the extract before adding a base? I rather tought the ephedrine is present as various organic compounds. |
||||||||
Newton (Hive Bee) 04-03-04 09:58 No 498880 |
Ephedrine freebase is volatile, I was clear on | |||||||
Ephedrine freebase is volatile, I was clear on that. So what exactly was that oil you were talking about, then? rather tought the ephedrine is present as various organic compounds. What exactly are you referring to? 'Organic compound' is a rather large class of substances. You got some serious reading to do. HINT: Ephedrine will always be ephedrine, either in freebase form, or as a salt. There are other structually similar substances in the mix, however. This group would be called the ephedra alkaloids. L-Ephedrine is the dominant alkaloid in Ephedra extract- neither the freebase or any salts of it would look like an oil. They are crystals, at standard room temperature/pressure. Try to understand how acids/bases transform the ephedrine from freebase to salts, and vice versa. What impact would this have on the solubility in a polar solvent, like water? Now the idea is to get rid of the powder and the insolubles and thus the use of less solvent to improve handling. Extract with water first, filter and boil it off. You have obviously never tried filtering that stuff off. Its virtually impossible. Steam distill is the way to go, Soxhlet extraction probably works, but requires some fancy glassware. |
||||||||
jeffmills (Stranger) 04-03-04 11:42 No 498891 |
Re: So what exactly was that oil you were... | |||||||
So what exactly was that oil you were talking about, then? I was talking about the crude extract you get after destilling or evaporating off the alcohol. A sticky substance I might have falsely described as an oil. Ephedrine will always be ephedrine, either in freebase form, or as a salt. Yes, I fully agree. But in what form is the ephedrine present in the ephedra extract (or crude herb)? You have obviously never tried filtering that stuff off. Not when extracted with water. With alcohol just wait until the powder sinks to the bottom and then scoop off and filter the liquid. This may or may not work with water. Judging from a tea I've made from the ephedra extract several times I don't see any problems but I might err. If my previous posts were unclear I apologize. I hope everything is clear now. |
||||||||
biotechdude (Hive Bee) 04-04-04 02:00 No 498976 |
read more | |||||||
Yes, I fully agree. But in what form is the ephedrine present in the ephedra extract (or crude herb)? They are polyhydrates of a weak acid (prob water) or something like that. Neither freebase nor hcl salt persay; but complexes that dont allow them to be simply washed away with plain water (as the Hcl would), or an insoluble oil within the plant (as the freebase would). Thats why u need to convert it to one or the other and start extracting from that point on. If u want to do a water soak, do so on the powdered herb and add some hcl acid in so it converts to the hcl salt and hence increases its solubility. Then filter. Then base it up and NP extract or steam distill out the freebases. Then convert back to the salt and evap the water. If lucky, u will get salts that may be white. Further cleaning most probably will be necessary if u will be performing further reactions with it... Lastly, read some more posts from Dwarfer, Newton, Biotechdude and other Bees...u will get a better taste of what works... |
||||||||
jeffmills (Stranger) 04-04-04 05:25 No 498995 |
read more | |||||||
read more More reading certainly can't be wrong, but I guess I have read nearly all post concerning this matter. Most of them deal with the herb and not the extract. The extraction of the herb is somewhat more complicated, you have a lot of waxes, tars, plant matters and what not. Ephedra extract is a different story and thus there is no need for those fancy methods of getting the alkaloids out. It is straight foward: extract multiple times with alcohol, filter, destill or evap, add dH2o and NaOH, extract with np, wash np, dry and gas, recrystallize or just rinse with ice cold aceton. No gunk, no emulsions. This is probably as good as it gets. Sometimes a little powder is scooped up when filtering off the alcohol. When it dries up it is hard and looks glazed. (This is the unknown sticky 'oil' present in the ephedra extract.) It can't be washed off with alcohol but will readily dissolve in water. My conclusion is that the unknown 'oil' (presumably holding the alkaloids in whatever form) is very soluble in water and less soluble in alcohol in general. In addition the powder takes up a large quantity of solvent which is hard to get out unless you tie it up in a cloth and wind it out. So my idea to pre-extract with water is getting rid of the powder and all the water insolubles the alcohol pulls. Now is this unknown 'oil' volatile or not? Or more general: assume making a tea and covering a little powder with boiling water. If it was volatile no ephedrine would be left in your tea before drinking. I really do appreciate all your comments (except UTFSE), but no one could answer me this specific question yet. |
||||||||
biotechdude (Hive Bee) 04-04-04 06:14 No 499007 |
water, THEN alcohol extract | |||||||
Swix thinks he sees what you're getting at... So u 'wash' the plant with water to get of water solubles and small gunk. Then proceed with an alcohol extraction to get the goodies. Well, it may produce a 'cleaner' alcohol extract, but the actual alkaloid content would be low he presumes. This is because he has seen and used the black shiny tar like alcohol (only) extract, and results were poor. It did not dissolve well at all in water; indicating that not many water solubles were carried over (which you assume would be removed with a water wash). The water may indeed remove small bits of plant matter, and make your alcohol extract cleaner - but it will also remove some goodies (as in a tea)....but the main problem is that even then; the alcohol doesn't extract much goodies anyway. Then further cleaning needs to be performed where other problems with the a/b procedure (ephedrine freebase is soluble in water and the NP) and emulsions become apparent. If u wish to persue the alcohol path; a large Soxhelt could be constructed but good luck... |
||||||||
jeffmills (Stranger) 04-04-04 07:32 No 499017 |
Not sure if you got me right | |||||||
SWIM would wash the ephedra extract with water to make use of the great solubility of the unknown 'oil' holding the alkaloids in water and discarding the powder and all remaining insolubles. This step will pull the alkaloids and any water soluble gunk. Then boil off the water assuming the form of ephedra we are dealing with at this point is not volatile. (This is not clear to me yet.) The remaining black goo is then extracted with alcohol leaving the gunk and any other alcohol insolubles behind but we will not have any water insolubles either. So the remain should be soluble both in water and alcohol without any precipitate (which usually forms in alcohol only extractions after adding water to the black grease). Then proceed as aforementioned. The benefit (if the water boiling step does no harm) would be the small quantity of evaporation residue compared to the bulk mass of powder and therefore less alcohol can be used and result in better overall handling I guess. But that all depends on the volatility of the unknown 'oil' in the ephedra extract. If it is volatile the water pre-extaction would make no sense at all. The 'black tar' you describe should easily dissolve in water precipitating some water insolubles. |
||||||||
biotechdude (Hive Bee) 04-04-04 15:12 No 499064 |
comments | |||||||
But that all depends on the volatility of the unknown 'oil' in the ephedra extract. If it is volatile the water pre-extaction would make no sense at all. Swix powders his plant with dry ice, covers with pH 1 hcl/water mix, and heats to simmering for a few hours; then pulls. This is then repeated, but a thrid pull on the higher alkaloid % lines would also be necessary. That said, a plain water pull on the rough chopped plant just wouldn't cut it in Swix's book. You may need to take heed of his prior suggestions for greater effeciency. If you plan to boil down the water extract to dryness; Swix would recommend adding a little acid to ensure all the alkaloids are in their hcl salt form - and hence are not steam volatile. He says this as the sticky tarlike extract obtained by alcohol extract seems to indicate the composition of the alkaloids as they naturally occur in the plant; a halfassed mix of freebase and acids (that most probably be steam volatile to some extent; lowering yield somewhat more). Also, after u evap the water off and add the alcohol...how do you plan to remove it from the insoluble gunk left at the bottom? decant, filter? In conclusion, rather than plain water pulls - use a weak HCL pull (with powdered herb, heat etc if necessary), then evap to dryness (which is a bitch btw), then do alcohol pull, and proceed as normal.... Try it on a few kgs and see what happens, the herb doesn't cost alot in most places (except where Swix is ...) |
||||||||
jeffmills (Stranger) 04-04-04 15:57 No 499073 |
Trial and error | |||||||
Also, after u evap the water off and add the alcohol...how do you plan to remove it from the insoluble gunk left at the bottom? decant, filter? Decant and filter. In the end it depends on how viscous the gunk is. Either pre-filter through a cloth, rinse and wind it out or just wash and decant until no goodies are left and then discard as is. It has to be easier than the powder though which soaks up 1/2l solvent per kg roughly estimated. In conclusion, rather than plain water pulls - use a weak HCL pull (with powdered herb, heat etc if necessary), then evap to dryness (which is a bitch btw), then do alcohol pull, and proceed as normal.... Sounds good. SWIM will give it a try. Thanks for your input. |
||||||||
Newton (Hive Bee) 04-04-04 22:44 No 499132 |
But in what form is the ephedrine present in... | |||||||
But in what form is the ephedrine present in the ephedra extract (or crude herb)? Biotechdude has pretty much summed it up. General procedure is to either acidify or base the solution, to completely convert the ephedrine either into the freebase or the salt- depending on the polarity of the solvent you are going to employ. Please post your results of the planned water/ alcohol extraction. You will most not get white crystals after that procedure, as Ephedra contains some brown gunk, which is easily soluble in both water and alcohols. This stuff can be removed with recrystallisation however, which should be done anyway. |
||||||||
auntyjack (Hive Bee) 04-14-04 17:09 No 500874 |
what the! | |||||||
all info on ephedra alkaloids i've seen says they are in freebase form...so now i find out i've been chucking out half the goodies....alls well that ends well i guess.. also, the alky extract DOES have lots of water soluable shit in it and if you basify and wash in water to remove shit, the ephedrine that is lost with the water can be distilled out again...of course the distillation will give you some of the water soluable impurities back but plenty of crap is left behind also, there is NO NEED TO PURIFY THE ALKALOIDS down to a crystal or white powder except to keep the amount of reagents at a bare minimum....if you have litres of hi lying around (yeah sure) just react the raw alky sludge and steam distill the amphetamines at the end to avoid emulsions that would happen with an a/b.... the horror |
||||||||
sGv (Hive Bee) 04-25-04 07:38 No 502858 |
Pain in the ass .messed around with the raw... | |||||||
Pain in the ass .messed around with the raw herb tried for weeks to get something back besides green yack.. steaming worked a little better though but all and all not worth it ...swim will still be buying cases of e http://plaza-2000.cjb.net/ |
||||||||
place (Hive Bee) 04-25-04 11:29 No 502911 |
In conclusion, rather than plain water pulls - | |||||||
In conclusion, rather than plain water pulls - use a weak HCL pull (with powdered herb, heat etc if necessary), then evap to dryness (which is a bitch btw), then do alcohol pull, and proceed as normal.... When SWIM did a straight MeOH extract, he got a brown olie mass, which was absolutely imposseble to work with. Just so SWIM understand what you saying: Ligthly boil the plant in water pH > 1 a few hours, filter (will there be a lot of ephedrine in the discarded plant mass??), evap and collect raw crystals. Extract the raw crystals with alkohol, collect crystals and turn them to FB and then steam destil.? Or just do a straigth steam destil.? Actually should you maybie, be able to just react the raw crystals after water HCL + alkohol pull, following this link: ../rhodium /ephedra Flipside |
||||||||
biotechdude (Hive Bee) 04-26-04 16:25 No 503207 |
just steam distill | |||||||
You are adding steps that are not neccessary...u have an obsession with using alcohol. The best option is to steam distill either - A raw plant/NaOH solution The based up HCL extract Then titrate the freebase ditillate to 6 and u will get fluffy white salts. Then recrystalise using water/acetone for Mr-Sparkilo crystals No alcohol, filtering required... |
||||||||