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    Old 09-08-07, 01:08   #1 (permalink)
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    acid base extraction of poppy pods?

    just curious if someone tried one of the proven acid/base teks for DMT and Cacti on poppy pods.

    anyone ?
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    Old 10-31-07, 17:12   #2 (permalink)
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    a foaf did a hot water extract on dried poppy powder and then defatted that with toluene and yielded a fine tanninsh brown powder thats strong as shit. how does this method sound to the experts?
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    Old 10-31-07, 19:46   #3 (permalink)
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    Don't work. Look up the ph my friend. The best method is published in an easily obtainable (google) dea document from several years back.
    Better yet, the Merck Index answers a shitload of questions in this forum.
    Just a reminder, look into scheduled chems before you attempt to attain and DO NOT buy them online.
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    Old 10-31-07, 20:37   #4 (permalink)
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    what scheduled chems were you referring to?
    i dont see why it wouldnt work, if you can make tea out of poppy that means opium is polar, so adding a non polar solvent wouldnt remove any of the goods. care to explain to me why it wont work? there is no basication so the opium should be polar throughout the whole process.
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    Old 10-31-07, 21:24   #5 (permalink)
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    I thought opium is only the gooey latex scraped from the pod...?
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    Old 10-31-07, 21:32   #6 (permalink)
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    SWIMS AB extraction of poppy pods was a total disaster. none, nada, nothing ...
    dunno why it didn't work for poppy alkaloids.
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    Old 10-31-07, 21:42   #7 (permalink)
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    i am not proposing an AB extraction, there is no basification. just a hot water extract that is then defated with toluene and evapped.
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    Old 11-01-07, 02:25   #8 (permalink)
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    You seem to be shooting for morphine here. And you're on the right track. I was replying to the first post.
    As for the chems, acetone, MEK, and several others are scheduled right now. No shit. It's right on the shelf @ Home Depot, but scheduled...I don't get it either, if you can walk right up & buy it. I always thought scheduled meant they want id, atleast. Probably won't be long. I do know certain combinations of things set off alarms, such as buying a hot plate, lye & cold pills @ WalMart brings the police immediately. Also, if you have uninvited guests & they see the solvents & no paint uncomfortable questions will be asked.
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    Old 11-01-07, 20:26   #9 (permalink)
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    Acetone?! Are you fucking kidding me?

    Damn
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    Old 11-02-07, 14:25   #10 (permalink)
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    Tone is very much a listed precursor chemical.
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    Old 11-02-07, 15:01   #11 (permalink)
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    listed and or watched is MUCH
    different from scheduled
    there are what are called thresholds for listed or watched chems
    if youm buy more than a certain amount
    and it can be cucmulative
    then you must provide documentation (drivers license etc) to obtain hte chem
    acetone mek toluene xylene iodine hcl
    are all watched
    red p and hi are scheduled
    meaning you need a license to own them
    remember soem chems have a threshold of ZERO
    meaning that ANY amount to be purchased requires
    documentation
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    Old 11-05-07, 17:54   #12 (permalink)
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    Matchbooks are in common circulation, so your "any amount" theory is out the window for rp. Some of that which you refer is thresholds for export. Don't know what "hi" is.
    I do know what precursor chemicals are as far as the charge is concerned. I'm far from a chemist and I'm the first to SCREAM it on any public forum. Just trying, as far as my limited knowledge goes, to keep people safe, not split hairs.
    Anyone buying questionable items on their own ID pretty much has it coming imo.
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    Old 11-05-07, 23:41   #13 (permalink)
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    hi= hydroiodic acid?
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    Old 11-06-07, 08:02   #14 (permalink)
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    Quote:
    Originally Posted by NEPHROSIS View Post
    hi= hydroiodic acid?
    Learn something everyday
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    Old 11-08-07, 18:26   #15 (permalink)
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    Morphine is a zwitterion, it is soluble in both acidic and basic solutions. In order for morphine to not be water soluble, for the morphine to precipitate out and also be solvent extractable, the solution has to be around pH 9.1. Also morphine is not soluble in chloroform and presumably dichloromethane. I'm not sure exactly what non water-miscible solvent morphine is reasonably soluble in, I'd try toluene first, and if that doesn't work then diethyl ether.

    The book "Opium Culture" 2006 by Peter Lee is an excellent book and explains why opium with all the various alkaloids (36 or so) combined are much better than morphine which is just one of the alkaloids you can pull out. This is the best book I've ever read on opium. Highly recommended.

    Morphine = 3 to 24 %
    Codeine = 0.4 to 1.0%
    Thebaine = 0.4 to 0.8%
    Papervine = 0.4 to 0.8%
    Narcotine = 4.0 to 7.0%
    Narceine = 0.2 to 0.5%

    Opium is a complex cocktail of active alkaloids, the effects of which work in complementary synergy. For every negative side effect caused by one alkaloid there is another alkaloid with opposite properties to counteract that effect and establish overall balance. Thus it is the sum total of all the essences and energies in opium, working together in synergistic and complementary concert, that gives the Big Smoke its unique character and creates such a smooth harmony of effects in the human system. The net effect produced by this balanced blend of alkaloids when taken together in whole opium is completely different from and far less harmful to the human system than the effects caused by any one of its constituent alkaloids taken alone. Morphine and heroin, for example, have all sorts of dangerous side effects for the habitual user--including chronic constipation, impaired digestion, depressed respiration, sluggish circulation, and diminished alertness--and they contain no other alkaloids with complementary properites to counteract these hazards.

    Opium, however, in which morphine usually constitutes less than ten percent of the active components, contains codeine and papaverine to stimulate the bowels and counteract morphine's constipating effects, narcotine to accelerate respiration and counterbalance morphine's inhibitory influence on breathing, papaverine and other vasodilators to increase blood flow and offset morphine's suppressive influence on circulation, and thebaine to stimulate the brain and counteract morphine's soporific effects. Both physiologically and psychologically, the way opium influences the human system is therefore totally different from morphine, codeine, or any other fractional isolate of opium, and consequently opium addiction results in very different behavioral patterns compared with addiction to morphine or heroin.
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    Old 11-09-07, 16:30   #16 (permalink)
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    wait, so could goodies be lost in the toluene defat?
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    Old 11-09-07, 17:05   #17 (permalink)
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    i had once posted this...but it was purely hypothetical ---

    based on the fact that morphine is a naturally occuring alkaloid (from a plant like caffeine in tea leaves or coffee beans)---- we can see that water is an effective way of extracting the morphine, just like we extract the caffeine from tea leaves...... (and take nothing away from hips yogurt tek, that is a great method)----- but recently i have been toying with the idea of extracting the alkaloids just like we would extract caffeine in the lab --- for the case of pods....i have considered boiling them with a base such as sodium carbonate for around 30 minutes, at which point we would filter out the pod-matter, place liquid in a test tube (or centrifuge tube--- not so likely at home) and add some (4-5) portions (size dependent on amount of pod matter/water used) of an organic solvent such as methylene chloride.......each of these portions will be added singularly, mixed or centrifuged....then the lower phase would be removed, and then portion #2 of the solvent would be added, mixed....and then the lower phase removed until all 4 portions are completed ---- the lower phases of liquid that will have been removed would be placed into the same flask or container -----then sent through a pipet or similar drying tube constructed of: glass wool in the neck and some sodium sulfate on top the glass wool (to dry out the extract)............the "dried" extract would then be gently heated in a sand bath or similar to evap. the methylene chloride out leaving us morphine crystals ---- but then we would have to purify these relatively pure morphine crystals with ethanol (prob 95%) to remove the excess methylene chloride (which we dont want to ingest) completely ---- (however this is a somewhat more complex mechanism) ---- but the end result should give us pure morphine crystals ----

    -----

    either way i think i would use water first.....then the solvent of choice.....

    and note this is just something i thought up and have had no time to put any energy in to since then....

    lot of chem on the boards lately....Good Stuff!
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    Old 11-09-07, 18:42   #18 (permalink)
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    if poppy powder is acidified with vinegar (as oposed to basified with sodium carbonate) and defatted with toluene what happens to the morphine?
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    Old 11-11-07, 22:58   #19 (permalink)
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    To theoretically extract morphine, you need to boil the powdered pods in water, then filter. Raise the pH to 9.1 with sodium hydroxide solution then extract with toluene. Extract at least 6 times, each time making sure the water is still at pH 9.1. Morphine only precipitates out of the water at pH 9.1, below pH 8.9 and above pH 9.3 it's water soluble. But even at pH 9.1 about 1 gram per Litre can stay in the water. So multiple extractions are needed. The toluene can then be distilled off to leave the morphine and other opiate alkaloids in their smokable freebase form.

    ---------------------------------------------------------------------------

    Maybe you should give this recipe from poppies.org a try. The end result of this simple vodka tincture is a laudanum that is so strong you'd probably only need a tablespoon of it to get off. Everybody there says it doesn't degrade either, which sounds nice.

    For Those Still Drinking Poppy Tea... - Somni-Forum

    The idea is a soak and strain of poppy powder, decant then use the same alcohol to soak and strain even more poppy powder thus doubling the strength. Using his ratios you end up with a tincture that has the morphine equivalent of 6.5 grams of poppy pods in every tablespoon. If you still don't have enough potency just evaporate some of it.

    Everyone in the thread who's tried it are like ***damn it hits hard and fast.

    Myself, I love kratom and don't mess with poppies or pills anymore.

    -----------------------------------------------------------------------------

    Process for extracting and purifying morphine from opium

    Abstract

    A process for extracting morphine from opium is described. In the process, opium is extracted with a basic alcoholic solution. The basic alcoholic solution is filtered and the alcohol removed from the filtrate to leave a residue. The residue is then extracted with a basic aqueous solution having a pH of at least 11. The basic aqueous solution may be filtered to remove any solid matter remaining after the aqueous extraction step, and then be stirred with a sufficient amount of a salt to avoid emulsion formation. The basic aqueous solution or filtrate is then extracted with benzene or toluene. Next, adjusting the pH of the basic aqueous filtrate to pH 8.5 to 9.5 allows the morphine to precipitate and be recovered.
    Inventors: Ma; Junning (North Wales, PA); Corcoran; Robert C. (Laramie, WY)
    Assignee: The Board of Regents of the University and Community College System of (Reno, NV)
    Appl. No.: 753061
    Filed: November 19, 1996

    Current U.S. Class: 546/44
    Intern'l Class: C07D 489/00
    Field of Search: 546/44
    References Cited [Referenced By]
    U.S. Patent Documents
    1048712 Dec., 1912 Lloyd 546/44.
    2715627 Aug., 1955 Mehltretter et al. 546/44.
    Foreign Patent Documents
    189439 Jan., 1966 RU 546/44.
    1 80 189 Oct., 1935 CH 546/44.
    457 433 Nov., 1936 GB 546/44.
    750359 Jun., 1956 GB 546/44.


    Other References

    Loeffler. Chem Abstr vol. 62, Entry 11640 b abstr. DD 28733, 1965.
    Trojanek, Chem Abstr vol. 98 Entry 81d0 abstr Czech 197403, 1982.
    Bentley Chemistry of the Morphine Alkaloids, Oxford, Clarendon Press, p. 16, 1954.

    Primary Examiner: Shah; Mukund J.
    Assistant Examiner: Sripada; Pavanaram K
    Attorney, Agent or Firm: Morgan, Lewis & Bockius LLP
    Parent Case Text


    This application claims the benefit of the filing date of U.S. provisional application Serial No. 60/007,418 filed Nov. 21, 1995.
    Claims


    What is claimed is:

    1. A process for selectively extracting morphine from opium, comprising the steps of:

    extracting opium with a basic solution of a C.sub.1 -C.sub.6 alcohol capable of dissolving morphine in its neutral, cationic, or anionic form,

    filtering the alcohol solution,

    removing the alcohol from filtrate to leave a residue,

    extracting the residue with a basic aqueous solution having a pH of at least 11,

    optionally filtering the basic aqueous solution to remove any solid matter remaining after the aqueous extraction step,

    optionally stirring the basic aqueous solution with a sufficient amount of a salt to avoid emulsion formation,

    extracting the basic aqueous solution with a substantially water-immiscible organic solvent to remove non-morphine alkaloids from the solution,

    adjusting the pH of the basic aqueous filtrate to pH 8.5 to 9.5 to precipitate morphine, and

    recovering the morphine.

    2. A process of claim 1, comprising the steps of:

    extracting opium by refluxing in a basic methanol solution having a pH of about 9,

    filtering the methanol solution to remove any particulate matter remaining from the methanol extraction,

    removing the methanol from filtrate to leave a residue,

    extracting the residue with an aqueous solution of alkali hydroxide having a pH of at least 11,

    optionally filtering the basic aqueous solution to remove any solid matter remaining after the aqueous extraction step,

    optionally stirring the basic aqueous solution with a sufficient amount of a salt selected from lithium chloride, lithium bromide, lithium acetate, sodium chloride, sodium bromide, sodium acetate, potassium chloride, potassium bromide, and potassium acetate, to avoid emulsion formation,

    extracting the basic aqueous solution with a substantially water-immiscible organic solvent selected from benzene, toluene, xylene, diethyl ether, chloroform, and mixtures thereof, to remove non-morphine alkaloids from the solution,

    adjusting the pH of the basic aqueous filtrate to pH 8.5 to 9.5 to precipitate morphine, and

    recovering the morphine.

    optionally filtering the basic aqueous solution to remove any solid matter remaining after the aqueous extraction step,

    optionally stirring the basic aqueous solution with a sufficient amount of a salt selected from lithium chloride, lithium bromide, lithium acetate, sodium chloride, sodium bromide, sodium acetate, potassium chloride, potassium bromide, and potassium acetate, to avoid emulsion formation,

    extracting the basic aqueous solution with a substantially water-immiscible organic solvent selected from benzene, toluene, xylene, diethyl ether, chloroform, and mixtures thereof

    adjusting the pH of the basic aqueous filtrate to pH 8.5 to 9.5 to precipitate morphine, and recovering the morphine.

    3. A process of claim 2, further comprising, before the extraction step of extracting with a substantially water-immiscible organic solvent, the steps of:

    filtering the basic aqueous solution to remove any solid material remaining after the aqueous extraction step,

    stirring the basic aqueous solution with a sufficient amount of sodium acetate to avoid emulsion formation; and

    filtering the resulting solution.

    4. A process of claim 2 further comprising, after filtering the methanol solution, the steps of:

    extracting the particulate material a second time by refluxing in a second basic methanol solution having a pH of about 9,

    filtering the second methanol solution to remove any particulate matter remaining from the methanol extraction, and

    combining the second methanol filtrate with the first methanol filtrate for use in the methanol removal step.

    5. A process of claim 1, wherein extracting step refluxes opium in a basic solution of an alcohol selected from methanol, ethanol, isopropanol, and mixtures thereof, and having a pH of about 9; and wherein the substantially water immiscible solvent is selected from benzene, toluene, xylene, diethyl ether, chloroform, and mixtures thereof.

    6. A process of claim 5 further comprising, after filtering the methanol solution, the steps of:

    extracting the particulate material a second time by refluxing in a second basic alcohol solution having a pH of about 9,

    filtering the basic second alcohol solution to remove any particulate matter remaining from the alcohol extraction, and

    combining the second basic alcohol filtrate with the first alcohol filtrate for use in the alcohol removal step.

    7. A process for selectively extracting morphine from opium, comprising the steps of:

    extracting opium with a basic solution of methanol,

    filtering the methanol solution,

    removing the methanol from filtrate to leave a residue,

    extracting the residue with a basic aqueous solution having a pH of at least 11,

    optionally filtering the basic aqueous solution to remove any solid matter remaining after the aqueous extraction step,

    optionally stirring the basic aqueous solution with a sufficient amount of a salt to avoid emulsion formation,

    extracting the basic aqueous solution with a substantially water-immiscible organic solvent to remove non-morphine alkaloids from the solution,

    adjusting the pH of the basic aqueous filtrate to pH 8.5 to 9.5 to precipitate morphine, and

    recovering the morphine.
    Description


    FIELD OF THE INVENTION

    This invention relates to an improved process for the extraction and purification of morphine from opium. The object of this invention is to provide a more economical method of preparing morphine that utilizes less environmentally toxic solvents.

    BACKGROUND

    Morphine is useful as an analgesic drug. It is also used as the starting material for the preparation of codeine, which is another analgesic and antitussive drug. Morphine occurs naturally in opium to the extent of 9 to 17% by weight, depending upon the opium source.

    There are many alternative methods of extracting and purifying morphine from opium. However, these methods suffer from several disadvantages, such as prolonged extraction times, low efficiencies and the involvement of hazardous chemicals such as chloroform and sulfur dioxide. What is needed is a cost-effective process which does not require large amounts of potentially toxic or hazardous solvents. When viewed from this perspective, none of the current methods are entirely satisfactory.

    Generally, current methods extract the alkaloids present in opium with either water or an acidic (e.g. oxalic acid) solution. Due to the limited solubility of the alkaloids in aqueous solutions, the extract is very dilute. This results in a large amount of the aqueous extract. Recovery of the alkaloids from the aqueous extract also requires large amount of organic solvents. The process is also lengthy and labor intensive. One batch of opium generally needs to be extracted four times over a period of four days for complete recovery of the alkaloids. Separation and purification of morphine from the other alkaloids in the aqueous extract is also time consuming and relatively complicated due to the physical properties of the extract and the nature of the substances present.

    SUMMARY OF THE INVENTION

    The present invention relates to a process for extracting morphine from opium. The process of the invention answers the deficiencies of prior art processes. In the process, opium is extracted with a basic alcoholic solution. The basic alcoholic solution is filtered and the alcohol removed from the filtrate to leave a residue. The residue is then extracted with a basic aqueous solution having a pH of at least 11. The basic aqueous solution may be filtered to remove any solid matter remaining after the aqueous extraction step, and may then be stirred with a sufficient amount of a salt to avoid emulsion formation. The basic aqueous solution is then extracted with a substantially water-immiscible solvent such as benzene or toluene. Next, adjusting the pH of the basic aqueous solution to pH 8.5 to 9.5 allows the morphine to precipitate and be recovered.

    BRIEF DESCRIPTION OF THE FIGURE

    FIG. 1 depicts a preferred process according to the invention for extracting and purifying morphine from opium.

    DESCRIPTION OF THE INVENTION

    According to the invention described herein, morphine is extracted from opium by stirring and/or heating, or preferably refluxing, opium in a basic solution of an alcohol, preferably methanol at about pH 9. The pH may be adjusted by the addition of an inorganic base (alkali hydroxide, or carbonate), ammonia, and the like. Preferred inorganic bases include, but are not limited to, sodium hydroxide and potassium hydroxide. After the extraction is complete, the alcohol extract is filtered to remove the undissolved particulate matter. The alcohol itself is then removed from the extracted alkaloids, preferably by evaporation under reduced pressure. The resulting residue, which contains the alkaloids, is mixed or extracted with an basic aqueous solution having a pH of at least 11, preferably an aqueous solution of an alkali hydroxide. This converts the morphine free base present into its anionic (morphinate) form which is soluble in basic solutions at pH values of 11 or above. Other opium alkaloids are relatively insoluble and, in general, at least partially precipitate out of the basic aqueous solution. After removing any precipitate, preferably by filtration, the remaining alkaloids are separated from the morphine-containing basic aqueous solution by extraction with a substantially water-immiscible solvent, such as toluene or benzene. Finally, the morphine free base is precipitated out of the resulting aqueous solution by adjusting the pH of the aqueous filtrate to pH 8.5 to 9.5. Preferably, the pH to precipitate the morphine ranges from about 9 to 9.3, and most preferably is about 9.1. This is accomplished by adding either an organic acid or a mineral acid. The yield and purity of morphine produced by this procedure are economically satisfactory. The morphine obtained from this process may then be further purified by known methods or utilized directly in a further process to convert it into codeine.

    As discussed above, the extraction of morphine from opium may be accomplished by stirring and/or heating, preferably refluxing, opium with a basic solution of an alcohol capable dissolving morphine in its neutral, cationic, and/or anionic form. Preferably, the alcohol is a C.sub.1 -C.sub.6 alcohol. Particularly preferred alcohols include methanol, ethanol, and isopropanol. Mixtures of alcohols may also be used. Methanol, the preferred solvent for the invention, is a excellent solvent for extracting alkaloids from opium. Almost all of the alkaloids, especially morphine, are highly soluble in methanol. Advantageously, the alkaloids are soluble in methanol in their neutral, cationic, or anionic forms. The addition of an alkali, alkaline earth, or other suitable base to adjust the pH of the alcohol, to about 9, makes the extraction process more efficient. This results in more alkaloids and less impurities being extracted into the alcohol. Refluxing opium in a basic solution of the alcohol, preferably methanol at about pH 9, for approximately one to two hours extracts more than 90% of the morphine present. In a preferred embodiment, 5 g of opium, cut into small pieces, may be extracted by reflux with 0.2 to 0.6 g, preferably 0.4 g, of sodium hydroxide in 25 ml of methanol for 1 to 2 hrs.

    An additional extraction of the opium with a basic alcohol, such as methanol at pH 9, can recover essentially all of the alkaloids from opium. The second extract can either be combined with the first extract or can be used to extract another batch of opium. Separation of the alcohol extract from the undissolved residue by filtration or other similar means is generally easy and fast. Unlike an aqueous extraction process, the assistance of filter aid at this step is generally unnecessary.

    The removal of alcohol by distillation, under reduced pressure, at elevated temperatures, or by other known techniques is much easier and more rapid than the concentration of aqueous extracts or organic solutions (e.g. toluene) usually required in prior art methods. A small amount of filter aid may be added to the alcohol extract before distillation to prevent the alcohol extract from foaming and bumping. As another advantage, the recovered alcohol, particularly methanol, can be recycled and used for another extraction without further purification.

    In the prior art extraction methods, morphine is usually kept as an acid salt due to concerns regarding the stability of morphine in basic solutions. To test the stability of morphinate in basic aqueous solutions, morphinate was analyzed by High Performance Liquid Chromatography (HPLC) and then allowed to stay overnight at room temperature. The morphinate was then reanalyzed by HPLC. No loss of morphine was found.

    According to the invention, the residue remaining after removing the alcohol is then extracted with a basic aqueous solution having a pH of at least 11. Preferably, the basic aqueous solution is a solution of an alkali hydroxide such as sodium hydroxide or potassium hydroxide. Solutions of other bases may also be used. Maintaining the pH of the aqueous extract at this pH and preferably within a relatively narrow preferred range allows high quality morphine to be obtained with good recovery. At lower pH values, greater amounts of morphine may be lost in the initial precipitate. At higher pH values, less impurities may be extracted into toluene. Maintaining the pH in the range of 11.5 to 11.9 is, therefore, preferred.

    The basic aqueous solution may optionally be filtered to remove any solid material remaining after the aqueous extraction step. Filtering the basic aqueous solution at this point removes insoluble non-morphine alkaloids. Any precipitate may be washed with an additional quantity of the basic aqueous solution to ensure increased recovery of the morphine.

    The basic aqueous solution or filtrate, if filtered, is then extracted with a substantially water-immiscible organic solvent to remove the remaining alkaloids from the basic aqueous filtrate. Suitable solvents include, but are not limited to, benzene, toluene, xylene, diethyl ether, and chloroform. Separation of the resulting aqueous and organic phases may be accomplished by techniques known in the art.

    Theoretically, non-morphine alkaloids are supposed to precipitate out of concentrated aqueous solutions at pH values around 11-12. However, the presence of concentrated morphinate ions may increase the solubility of the other alkaloids. Thus, substantial amounts of non-morphine alkaloids may remain in solution. Direct extraction of the basic aqueous solution or filtrate, if filtered, with a substantially water-immiscible solvent can remove those alkaloids, but may result in formation of an emulsion. To avoid emulsion formation, the aqueous solution/filtrate may, before extraction with the substantially water-immiscible solvent, first be treated with a sufficient amount of an alkali metal salt or alkaline earth metal salt, for example 0.5 to 5 grams salt for each 5 grams of opium. Preferred salts are, for example, lithium chloride, lithium bromide, lithium acetate, sodium chloride, sodium bromide, sodium acetate, potassium chloride, potassium bromide, or potassium acetate. A preferred amount of the salt is 0.5 to 2 grams per 5 grams of opium. Sodium chloride and sodium acetate are preferred salts with sodium acetate being particularly preferred. The extract may then preferably filtered again to get rid of any gummy or other precipitate prior to extracting with a substantially water-immiscible solvent, such as benzene or toluene.

    The sequence of the morphine purification procedure may, however, affect the recovery of morphine. For example, if, to avoid emulsion formation upon extraction, a salt is added to the basic aqueous solution before it is filtered after the aqueous extraction step, as much as about 20% of the morphine may precipitate out along with the other alkaloids. Accordingly, the recovery of morphine will be substantially lower.

    When extracting the aqueous solution/filtrate with a substantially water-immiscible solvent, such as toluene or benzene, a small amount, generally about 8%, of the morphine may be extracted into the solvent. This may be recovered by back extraction with additional basic solution, for instance, a sodium hydroxide solution. Any loss of morphine in the aqueous mother liquor, about 2%, may be recovered by additional extraction with the solvent. For health reasons, the use of toluene is preferred, particularly over benzene, in the process of the invention.

    Any alkaloids precipitated on a filter aid or paper in the process may be recovered by extraction with an alcohol, preferably methanol. The filter aid can be used again without further purification. The other opiate alkaloids that were extracted into the substantially water-immiscible solvent may be combined with the alkaloids which precipitated from the aqueous extract at pH 11.5 to 11.9 and further purified by other known methods.

    After extraction with the substantially water-immiscible solvent, the pH of the basic aqueous solution/filtrate is adjusted to about 8.5 to 9.5 to precipitate the morphine. Preferably, the pH is adjusted to 9 to 9.3 and more preferably to 9.1. The pH may be adjusted using an acid such as, for example, sulfuric acid, hydrochloric acid or acetic acid. Preferably, a 50% acetic acid in water solution is used.

    The precipitated morphine may then be recovered using techniques known in the art such as filtration or decantation. The recovered morphine is preferably washed with water before drying.

    The foregoing procedure provides a cost-effective process for isolating morphine from opium. This procedure provides good recovery and a high quality product FIG. 1 depicts a preferred process of the invention. The whole process, from extraction of opium to precipitation of purified morphine, can generally be completed in one day. This is much more efficient than other existing commercial purification methods.

    The following specific example illustrates the invention, but is not intended to limit the scope of the invention.

    EXAMPLE

    5 g of opium were cut into small pieces and extracted by reflux with 0.4 g of sodium hydroxide in 25 ml of methanol for 1 to 2 hrs. The methanol extract was then filtered to remove particulate materials. After addition of 1 g of filter aid to the methanol extract, which contained 465 to 485 mg of morphine, the methanol was removed under reduced pressure. The residue was then mixed with 5.5 ml of 1.0 N sodium hydroxide solution at 35.degree. C. for 10 min. and the pH adjusted to about 11.5 to 11.9 with 50% acetic acid in water. This aqueous extract was then filtered and the precipitate washed with 5.5 ml of 0.01 N sodium hydroxide solution. The combined aqueous filtrate was stirred with 0.5 g of sodium acetate for 10 minutes and filtered again. The filtrate was then extracted twice with 5 ml of toluene and the pH of the aqueous filtrate was then adjusted to pH 9.1, with 50% acetic acid in water. The mixture was allowed to remain for a period of 6-10 hrs at room temperature for complete precipitation and was then filtered. This precipitate was washed with water and dried at room temperature. This final precipitate contained 400-426 mg of morphine, which represented a recovery of 86-88% based upon the amount of morphine in the initial methanol extract. The purity of morphine following this procedure was 84% to 86% by weight.
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    Old 11-12-07, 12:25   #20 (permalink)
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    excellent info tregar ---good to know i wasnt too far off

    the toluene is the best part as it is not carcinogenic like the methylene chloride so no extract purification needs to be accomplished

    very nice!
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    Old 11-12-07, 14:48   #21 (permalink)
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    Excellent discussion Python, no you were not far off at all!
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    Old 06-09-08, 19:19   #22 (permalink)
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    Boilling MeOH is very effective at stripping pods of alkaloids. If you soaked\washed the pods in an appropriate defatting solvent, and then dry them, you could probably get a pretty potent extract.

    Boiling MeOH alone extracts a lot of crud, but it is much easier to consume.

    This stuff is a tad more complicated to issolate than DMT or Mescaline. As I am sure you have noticed, it takes a lot less pods eaten straight to get you where a tea will. This is, of course, due to the reluctance of these compounds to move where you tell them.
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    Old 06-09-08, 19:39   #23 (permalink)
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    just go home from work and i'm really tired so i didn't read everything. if you basify with say naoh all the alkaloids EXCEPT morphine (the one you really want) will go base. this is good to remove everything but the morphine. to get the morphine to go base you need to use calcium "something" like i said i'm bushed right now and i forget what calcium base you need. once the morphine is in the base form you can extract as usual.
    a foaf did it once AND had some aa. i got to do some of the result and was very pleased.
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    Old 06-09-08, 20:06   #24 (permalink)
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    I hear a relatively easy method for clean(ish) freebase alkaloids can be had by the following:

    -take your ground/powdered pods and soak in water/vinegar solution... (like making normal tea, but with 50/50 water/white vinegar)

    -filter out pod ground

    -add ammonia (normal store bought)....use a liberal amount(solution should go white cloudy)....let sit undisturbed for an hour

    your morphine and some other alkaloids will present themselves as the top layer (middle layer will be mostly water and a bottom layer of organic/mineral solids will also precipitate)

    decant off top layer and evaporate

    resulting material is smokable


    sorry I dont have actual figures for the amounts
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    Old 06-11-08, 12:06   #25 (permalink)
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    I wish I could easily make oxycodone from pods heh
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    Old 06-13-08, 19:07   #26 (permalink)
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    $w!m thinks ice-cold filtering works, the simmered tea is first filtered to a fine brown liquid & placed in a container then into the freezer a few hrs until ice forms a layer around the tea solution, a small hole is poked thru the ice layer & the tea is poured into another container & placed back into the freezer, discarding the ice from the first container, this is repeated until you end up with a few oz's of very dark potent tea. form there you could just drink or evap the tea to tar or experiment with chem extractions.
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    Old 06-16-08, 15:49   #27 (permalink)
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    Name:  cp2.bmp
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Size:  506.3 KBHi, im new here and have a few questions. i recently came across some somniferum flowers around 15 or more and was wondering if the pods were edible as is for effects or is it mandatory to extract the alkaloids by making tea to prevent some sort of poisoning. im no lightweight but im no chemist eather so i figure asking before i do something i may regret later.
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    Old 06-16-08, 16:16   #28 (permalink)
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