I tried to find a way to extract morphine and codeine nearly in it's pure form. So here is my extraction process which is build on simple a/b extraction which is used on opium to extract morphine.
I hope that it is okay that i made a new topic for it because i didn't want to resurrect an old topic. Also the reference is this extraction http://opioids.com/jh/index.html so i hope everything is right.
the extraction:
I would use 2 liter of water to extract 250g pulverised poppy pods. This solution will be acidified with hydrochloric acid to pH 2-3. Then it has to get stirred over night. So this should make all the alkaloids to their salt form, which dissolve in the water. After this it has to be filtered several times to get all the plant material out of the solution.
Now the whole filtrate has to get basified to a pH of 8-9 because in a basic medium the alkaloids are much more stable against high temperatures than in a sour medium. Also the pH is not high enough to deprotonate the Morphine alkaloid. Now nearly 90-95% of the solution can be evaporated and must be stirred at max. 80°C with a stream of dry air over it to evaporate faster. This stream can be made by a fan.
After the most evaporated the solution has to get acidified again to a pH of 2-3 to get all the alkaloids back in solution. Now the solution should stay in the fridge over night. A lot of grey/brown sludge will appear and it has to be filtered off. This sludge contains oils, resins and so on. This sludge can washed with a few ml of acidified water to wash the remaining alkaloids out of the sludge.
Now there should be a concentrated solution of opiates with some impurities in there but not as much as the beginning solution. I would now try to extract the impurities with some petrolether to get a cleaner solution. So the solution has to be washed 3-5 times with 1/5 of the volume of the solution of petrolether and get seperated with a seperation funnel. Now it has to be washed 2-3 times with the same volume of DCM. This cleaning process is important because I supposed to extract at the end the codeine out of this solution with some DCM. But now at first I would bring the pH to 9-10(exactly 9,1 to get the morphine into the free base) and let it stand again over night in the fridge to let the morphine and some of the codeine precipitate. There should be a precipitate which can be filtered off. This precipitate will be air dried and than I want to seperate the codeine from morphine. So I would put the dry powder in some DCM which should dissolve the codeine but not the morphine. After 1/2 hour I would filter off the morphine which has to be dried again to get the crude morphine base and let the DCM evaporate to get the crude codeine base.
From the mother solution where the morphine was filtered off i would wash it several times with DCM to get all of the codeine out of it. This DCM would evaporate also and the residue would be added to the crude codeine base.
Now to purify the morphine base it has to be dissolved in some hot isopropanol to get a saturated solution. Now it has to be added half of the volume of petrolether to shrink the solubility of the morphine base. After the addition there should be some precipitate. Again half of the volume of petrolether should be added and the solution stay again in the fridge to cool down until everything is precipitated. This purifying process can be made several times.
to purify the codeine base it has to be dissolved in some dry DCM again and then some HCl gas is bubbled through it to precipitate the codeine hydrochloride.
Now I want to know if you have some clues or hints or maybe a better idea to extract or to purify it. Also I have a few questions because I read that codeine builds a hemihydrate in water which is soluble in water. So I asked myself if I basify the water and the morphine and codeine precipitate out would there be a chance that the codeine which wants to precipitate builds up a hemihydrate which brings it back in the solution. And if it is so will DCM extract it or not? and what if not? Also are 250g poppy pods out of a moderate climate enough to get some morphine and codeine out of it or should I try a larger amount?
Sorry if my english is bad, it's not my mother language. I hope that it is understandable.
I hope that it is okay that i made a new topic for it because i didn't want to resurrect an old topic. Also the reference is this extraction http://opioids.com/jh/index.html so i hope everything is right.
the extraction:
I would use 2 liter of water to extract 250g pulverised poppy pods. This solution will be acidified with hydrochloric acid to pH 2-3. Then it has to get stirred over night. So this should make all the alkaloids to their salt form, which dissolve in the water. After this it has to be filtered several times to get all the plant material out of the solution.
Now the whole filtrate has to get basified to a pH of 8-9 because in a basic medium the alkaloids are much more stable against high temperatures than in a sour medium. Also the pH is not high enough to deprotonate the Morphine alkaloid. Now nearly 90-95% of the solution can be evaporated and must be stirred at max. 80°C with a stream of dry air over it to evaporate faster. This stream can be made by a fan.
After the most evaporated the solution has to get acidified again to a pH of 2-3 to get all the alkaloids back in solution. Now the solution should stay in the fridge over night. A lot of grey/brown sludge will appear and it has to be filtered off. This sludge contains oils, resins and so on. This sludge can washed with a few ml of acidified water to wash the remaining alkaloids out of the sludge.
Now there should be a concentrated solution of opiates with some impurities in there but not as much as the beginning solution. I would now try to extract the impurities with some petrolether to get a cleaner solution. So the solution has to be washed 3-5 times with 1/5 of the volume of the solution of petrolether and get seperated with a seperation funnel. Now it has to be washed 2-3 times with the same volume of DCM. This cleaning process is important because I supposed to extract at the end the codeine out of this solution with some DCM. But now at first I would bring the pH to 9-10(exactly 9,1 to get the morphine into the free base) and let it stand again over night in the fridge to let the morphine and some of the codeine precipitate. There should be a precipitate which can be filtered off. This precipitate will be air dried and than I want to seperate the codeine from morphine. So I would put the dry powder in some DCM which should dissolve the codeine but not the morphine. After 1/2 hour I would filter off the morphine which has to be dried again to get the crude morphine base and let the DCM evaporate to get the crude codeine base.
From the mother solution where the morphine was filtered off i would wash it several times with DCM to get all of the codeine out of it. This DCM would evaporate also and the residue would be added to the crude codeine base.
Now to purify the morphine base it has to be dissolved in some hot isopropanol to get a saturated solution. Now it has to be added half of the volume of petrolether to shrink the solubility of the morphine base. After the addition there should be some precipitate. Again half of the volume of petrolether should be added and the solution stay again in the fridge to cool down until everything is precipitated. This purifying process can be made several times.
to purify the codeine base it has to be dissolved in some dry DCM again and then some HCl gas is bubbled through it to precipitate the codeine hydrochloride.
Now I want to know if you have some clues or hints or maybe a better idea to extract or to purify it. Also I have a few questions because I read that codeine builds a hemihydrate in water which is soluble in water. So I asked myself if I basify the water and the morphine and codeine precipitate out would there be a chance that the codeine which wants to precipitate builds up a hemihydrate which brings it back in the solution. And if it is so will DCM extract it or not? and what if not? Also are 250g poppy pods out of a moderate climate enough to get some morphine and codeine out of it or should I try a larger amount?
Sorry if my english is bad, it's not my mother language. I hope that it is understandable.
bentley_morphine_alkaloids.pdf
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