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chrigu
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Joined: 28 Mar 2005 |
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extraction from poppy straw
Wed Mar 30, 2005 12:08 am |
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Hi everybody, im new to the forum. i know the following is probably bothering to you. i study something totally different from (bio)chemistry and so some of the basics in chemistry are missing ... but maybe if you have a minute time ... and forgive my english, im not native english speaking ...
i would try to extract morphine from poppy straw. i did the following:
1. grinded 100 gr. of poppy pods to a fine powder (as fine as you can get it with a coffee mill)
2. added ca(OH)2 to that so that the liquid was about 2 cm over the straw level.
3. heated that up in a water bath at 60 - 70 C for 2 hours.
4. filtered it through a normal coffee filter.
5. extracted 2 more times from the used material with less liquid.
6. added a non-mineral acid (citric acid) to make the pH 5.5
7. evaporated it down at 50 C on a water bath until i had an amount i could handle.
8. added ethanol 15% of the liquids volume and raised the pH to 11.5 with ca(OH)2 and sodium carbonate. let it precipitate in a cool dark place 4 hours.
9. filtered this through a coffee filter.
10. added some ethanol (to compensate if there was any loss while it rested and during the filtration). added ammonium chloride to make the pH 9.1.
11. i let it rest for 24 hours in a cool dark place to let morphine and codeine precipitate out.
12. filtered it through a coffee filter and dried what i found in there.
It wasnt much and didnt seem to be morphine.
im wondering what i did wrong. I was thinking maybe i should have:
a) put an ether layer on the liquid during the longer rest-periods to minimize atmospheric oxidation
b) used a finer filter, maybe a buchner with mild vacuum.
c) rubbed the inner side of the glass with another piece of glass to assist precipitation when i let the morphine precipitate out
Can you help me with this?
Thank you
chrigu |
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IndoleAmine
Dreamreader Deluxe
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Sun Apr 03, 2005 11:36 pm |
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Quote: |
added ethanol 15% of the liquids volume and raised the pH to 11.5 with ca(OH)2 and sodium carbonate. let it precipitate in a cool dark place 4 hours.
9. filtered this through a coffee filter.
10. added some ethanol (to compensate if there was any loss while it rested and during the filtration). added ammonium chloride to make the pH 9.1.
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The only thing that precipitated was probably calcium carbonate and sodium citrate (or other way round?), since the morphine alkaloids are soluble in EtOH as free bases (and you did create the free bases when adding Ca(OH)2...)
Then you filter off the salts and discard the 15% EtOH filtrate? Or keep it? Anyway, the ethanol holds probably most of your morphine/codeine I would guess. So the alkaloids cannot precipitate...
Try the same thing without any EtOH, and it should work fine.....
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java
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Mon Apr 04, 2005 12:53 am |
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chrigu......this is how it's done in large scale , so extrapolate from here for your particular application..........java
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The following is a step-by-step description of morphine extraction in a typical Southeast Asian laboratory:
1. An empty 55-gallon oil drum is placed on bricks about a foot above the ground and a fire is built under the drum. Thirty gallons of water are added to the drum and brought to a boil. Ten to fifteen kilograms of raw opium are added to the boiling water.
2. With stirring, the raw opium eventually dissolves in the boiling water, while soil, leaves, twigs, and other non-soluble materials float in the solution. Most of these materials are scooped out of the clear brown 'liquid opium' solution.
3. Slaked lime (calcium hydroxide), or more often a readily available chemical fertilizer with a high content of lime, is added to the solution. The lime converts the water insoluble morphine into the water soluble calcium morphenate. The other opium alkaloids do not react with the lime to form soluble calcium salts. Codeine is slightly water soluble and gets carried over with the calcium morphenate in the liquid. For the most part, the other alkaloids become part of the residual sediment 'sludge' that comes to rest on the bottom of the oil drum.
4. As the solution cools, and after the insolubles precipitate out, the morphine solution is scooped from the drum and poured through a filter of some kind. Burlap rice sacks are often used as filters. They are later squeezed in a press to remove most of the solution from the wet sacks. The solution is then poured into large cooking pots and re-heated, but not boiled.
5. Ammonium chloride is added to the heated calcium morphenate solution to adjust the alkalinity to a pH of 8 to 9, and the solution is then allowed to cool. Within one or two hours, the morphine base and the unextracted codeine base precipitate out of the solution and settle to the bottom of the cooking pot.
6. The solution is then poured off through cloth filters. Any solid morphine base chunks in the solution will remain on the cloth. The morphine base is removed from both the cooking pot and from the filter cloths, wrapped and squeezed in cloth, and then dried in the sun. When dry, the crude morphine base is a coffee-colored powder.
7. This 'crude' morphine base, commonly known by the Chinese term p'i-tzu throughout Southeast Asia, may be further purified by dissolving it in hydrochloric acid, adding activated charcoal, re-heating and re-filtering. The solution is filtered several more times, and the morphine (morphine hydrochloride) is then dried in the sun.
8. Morphine hydrochloride (still tainted with codeine hydrochloride) is usually formed into small brick-sized blocks in a press and wrapped in paper or cloth. The most common block size is 2 inches by 4 inches by 5 inches weighing about 1.3 kilograms (3 lbs). The bricks are then dried for transport to heroin processing laboratories.
............as taken from http://opioids.com/jh/ |
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java
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chrigu
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Joined: 28 Mar 2005 |
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Mon Apr 04, 2005 3:45 am |
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thank you for the replies.
i know this thread at drugs-forum. i would do it in my (many ) former tries without ethanol. to me it also seemed strange that ethanol should assist precipitation (because of the solubility). but someone wrote he read it in a patent that ethanol should assist ... so i thought id give it a try.
what i did was adding the ethanol, raising to 11.5, waiting for precipitate to settle down, then filtering, discarding the filtered material and keep the solution with the ethanol. then i would precipitate from this at pH 9.1.
Strange that it doesnt work for me because it seems to be a rather easy process. but who knows what i do wrong with my poor chemistry knowledge... had i just listened better in school
of course i did this only theoretically. i was just so much into it that my thoughts seemed so realistic that i would write it down as if i had really done it...
also i read that KOH is preferred to sodium hydroxide because of its pKa. What does this mean? |
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stooge
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Tue Apr 05, 2005 12:13 am |
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hm, btw, is there a good method to get out the thebaine (and/or the other opiates) left over by this operation? |
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chrigu
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Joined: 28 Mar 2005 |
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Wed Apr 06, 2005 1:13 am |
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i can only repeat what i heard (makes the whole subject a little unscientific - sorry for that)
there definately are patents on the isolation of thebaine. the companies are going over to sythesize morphine, codeine and other opioids from thebaine (for which some p.som. strains high in thebaine have been breeded and are grown, in france for example). |
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THE MOON RULES --1
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"ornamental"
Tue Apr 12, 2005 4:31 am |
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I've seen "ornamental" dried poppy straws for slae before. Is there actually enough active morphine/codiene that you can get a final product? How much would be needed? |
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chrigu
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Joined: 28 Mar 2005 |
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Sat Apr 16, 2005 2:13 am |
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Quote: |
Try the same thing without any EtOH, and it should work fine.....
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I just heard that ethanol can assist the precipitation of salts in an aqeous ammonious solution.
When the morphine is extracted into ca(oh)2 it should be the morphine calcium salt. But when I add ammonia (from AmCl) and make the pH 9.1 - will the morphine still be in the salt form or is it already freebase then? I guess its freebase when it precipitates out, right? Will ethanol still assist?
Anyhow. I found the following on google, what do you think about it?
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What do you think about this?
Needed: ether, caustic soda, HCl, distilled H2O, Filter, something to
shake the things is (sep funnel or normal plastic bag)
Morphine is a tertiary amine.
The solubility of the free base in water is 0,2 g/L. The solubilty of
Morphine hydrochloride is 57 g/L.
1. Opium is shaked in a 01 -1 M HCl solution and Ether.
[ That is an aquoeus solution with HCl (0.1 - 1 %). That means all
three are put together and are shaken. The morphine hydrochloride goes
over into the aqueous phase (because of the HCl, which takes
everything that can be made a salt), while non-basic components go
over into the etherphase. ]
2. The aqueous excerpt is then neutralised with caustic soda solution.
By doing this the Morphinehydrochloreide becomes less soluable in
water again because of the pH. This way the morphine free base
crystallizes out.
3. This precipitate is filtered out of the solution with a fine
Buchner funnel and mild vacuum.
If one adjusts it for poppy straw one would have to get "opium" from
that first:
Before the shaking in ether and dilutet HCl one would just have to
make an alcoholic extract from the straw. Preffered is methanol i
guess but ethanol should work as well (one can just run an extra
extraction with the used material)
I found this method in a "test" for pharmacy students. I guess that
this method isnt found in patents because they usually go for
industrial production and because of this look for the cheapest and
less dangerous way (ether is extremely flammable)
Comments and corrections from the specialists would be great.
Thank you.
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chrigu
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re: extraction from poppy straw
Mon May 16, 2005 8:21 am |
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Ok. I gave up on extracting m from straw. Sucks. I did everyting correct:
extracting into ethanol
filtering very clean
ph 6.5 with hcl
filtering
toluene wash for fats etc.
ph 9.1 with carbonate
np was with ether
nothing put a gross salty substance that burned on the tongue ....
in theory the above of course |
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DrugPhreak
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re: extraction from poppy straw
Mon May 16, 2005 9:53 am |
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Extracting alkaloids from straw is a hassle and the alkaloid content is extremely low (~1mg per gram even for the most potent straw). Grow some poppies and when an ounce of dry opium (which requires 125-250 poppies depending on variety) has been obtained extract the morphine like so...
28gm of dry Opium is added to 350ml of distilled water in a beaker and placed on a hotplate. The temperature is slowly raised with stirring until the Opium fully dissolves. Then 7.5gm of calcium hydroxide is added slowly to the solution with a little stirring. It is removed from the hotplate and allowed to cool and then filtered (just about everything on the filter paper contains insolubles and other crap). The solution is placed back onto the hotplate and slowly heated to 82°C. A few seconds after this temperature is reached strong ammonia is added until pH 9.1 and the solution is taken off the hotplate and allowed to cool. It is left to sit for about 2 hours. After it's been sitting for a while Morphine base will start to precipitate out of solution. When precipitation is complete the solution is vacuum filtered and the Morphine is spread out to air dry. It can be used as is for an acetylation and this is normally done in many Heroin producing countries, but it really should be turned into the HCl and recrystallized.
Yield: ~2.5gm |
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re: extraction from poppy straw
Wed May 25, 2005 2:15 pm |
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In response to the last recipe above this post, I am asking where I can find an easy recipe to TURN this crude morphine into HCL form. There was this comment further above in the first recipe:
7. This 'crude' morphine base, commonly known by the Chinese term p'i-tzu throughout Southeast Asia, may be further purified by dissolving it in hydrochloric acid, adding activated charcoal, re-heating and re-filtering. The solution is filtered several more times, and the morphine (morphine hydrochloride) is then dried in the sun.
However, it doesnt say if it should be dissolved in pure Hcl or how much, how much activated charcoal should be added by ratio, and how long it should be reheated for before refiltering. Could we get some clarification there from someone in here?
I would really really like to try this because the soil in my State is incredibly fertile and would be superb for poppy growing, and I caretake for MSCONTIN addicts and who knows with the present world situation as it is today they could close the pharmacies tomorrow for all we know then it be the end for all of those ppl.
Thanks. But thanks even more for that last recipe on making 2.5 grams of the crude morphine base, that seems about as easy as baking a cake. |
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zub
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re: extraction from poppy straw
Sat May 28, 2005 6:38 pm |
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obtaining dry opium from poppies is no cake walk in itself; quite labor intensive. also, the amounts mentioned here a very unlikely with lancing the pods and collecting the goo.
which might make poppy straw extraction seem less hopeless, by comparison.
the pre-flowering plant can be juiced; best done just before the flowering occurs, when the bio-mass is at maximum. the plant contains all the morphine it will ever have at this stage, and looks like endive in a garden...not part of the golden triangle.
furthar extraction from the plant juice is possible thru a variety of methods.
also, the dried plant material (excluding seeds) can be made into a tea; dehydrated; and furthar extraction from the dry tea.
slicing ripe pods is very slow; very suspicious looking, and one is highly unlikely to get the amounts suggested in the above posts. |
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zub
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Wed Jun 01, 2005 10:32 am |
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it worries me to not be called on this bluff.
even if i'm correct, shouldn't someone bee arguing the point?
btw, opium poppies, of high potency, can be grown quite easily in the majority of the temperate climate of the eastern united states.
i can't think of a single vegetable that is easier to grow than poppies. they jump out of the ground in early spring, when rainfall is plenty and insects are just waking up.
they make a crap-load of seeds that are extra-easy to harvest, and are plenty good as a food.
extractions of the goods are some of the easiest chemistry we could ever hope to encounter. even easier than mescaline from san pedro cactus.
i dig poppies because of the easy food they make, including honey. bees love a fucking poppy, and will make honey from its nector.
this is a plant worth cultivating; like marijuana, even if you aren't interested in altering your state.
come the revolution, poppies will appeal to us as a food source more than a drug.
the nutritional attributes of the seeds rival sunflower seeds and sesame seeds, while beeing much easier to harvest without expensive machinery.
fuck morphine, unless you're in deep pain.
poppies are beautiful because of protein and honey.
no garden is complete without them. |
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loki
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Wed Jun 01, 2005 3:03 pm |
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morphine forms salts with bases and with acids. The method i have seen for isolating morphine entailed forming calcium morphinate, because of the difference of solubility of codeine and morphine in this state... i can't remember where i found it, probably poppies.org. I don't think there is a simple way to make both of them come out nicely. |
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