Jaw Clenching
Bluelighter
- Joined
- Feb 4, 2005
- Messages
- 551
I've been trying to gather all the information I can about Morning Glory Seeds. Most of the information available on the 'net seems pretty unreliable. Hopefully the people of this forum can help put together some useful and factual information on this topic.
One of my primary goals is to determine what chemical(s) present in the seeds cause the ill side-effects commonly associated with their ingestion. So far, I've found that some of the suggested are:
* Essential oils present in the seed pulp that can irritate the GI tract.
* Cyanogenic Glycosides present in the seed coating (similar to the ones in apple seeds) that produce many ill side-effects.
* Pesticide and/or fungicide present on the outside of the seed that may or may not come off with soap and water.
* And finally, the Ergot alkaloids themselves may actually cause many of the ill side-effects everyone wants to avoid.
There are quite a few crude extraction teks online. Most seem to be minimally effective. On another forum, there have been a few new extraction methods suggested:
Method 1:
This tek was suggested to be preformed outside on a cold night due do the use of hexane
Grind seeds into powder.
Place the powder in a glass bottle or flask with a tapered neck that is supported somehow (ring stand or similar).
Spray hexane into the bottle with the seed powder in it.
"it (hexane) is readily available in its purest of forms from any electronic store as an electronic cleaning agent."
Cover the top of the bottle with filter paper and place a rubber band around it to keep it on. Poke a small hole through the middle of it.
Invert the bottle and let the hexane spill into a pyrex baking dish.
The hexane should evaporate very quickly leaving behind a relatively pure extract that's active at ~10mg+.
Method 2
1) Finely grind seeds into a powder. Make sure to maintain a low heat and light environment. Be careful with the electric coffee grinders as the friction creates the heat we're desperately trying to avoid. Using a pepper mill would be a better option (much more physical labor though).
2) Prepare an acidic solution in a clean glass jar. I'd recommend using cold distilled water and a pure, food grade acid (tartaric, acetic, citric, etc). Aim for a pH of around 5. If one were to use a stronger acid, an ice bath may be necessary to keep the solution cool.
3) Put the seeds in the cold, acidic solution. Put the lid on the jar, and shake it for about 15-30 minutes. Any more would be a waste of time IMO.
4) Defat with your non polar solvent of choice (cooking oil is not a good choice). Since what we want is not soluable in non-polar solvents right now, and we're not going to evaporate it away, it's ok to use something like hardware store naptha. Basically this step consists of combining a non-polar solvent with our acidic solution, shaking the two in a jar for a few minutes, separate and discard the non-polar layer, repeat. A separatory funnel is almost required here (they're quite cheap on eBay, get a Pyrex one). The more thourough one is with this step, the less 'gunky' the end product will be.
5) After removing all non-polar solvents from the previous step, we should have the desirables in a more stable form, dissolved in the acidic solution with little if any 'fatty plant crap'. Add a to be determined amount of amylase to the solution. Put the lid on the jar and shake it for however long you think it'd take for the enzyme to do it's thing. Hopefully this will rid our solution of the terrible glycocides.
6) Filter out all seed matter as it is now useless to us.
Now there are two ways we could go from here:
----------------------------------------
7A-1) Heat the solution to 80'F. Stir for an hour or so. This should rid us of the HCN in the solution (I'm not even sure if this will work). It may also rid us of the desirable alkaloids. I really can't say how sensitive the salt forms of the alkaloids are.
7A-2) Drink the solution or store it in the fridge for a later time.
----------------------------------------
7B-1) Another way to go with this (more involved, but may be much more efficient) is to preform a full acid/base extraction. We're now back on step 5 with the filtered acidic solution. In a separate glass jar / beaker create a basic solution. I'd use a 5M NaOH solution in distilled water. Household ammonia and perhaps baking soda would work too. If the creation of the basic solution was exothermic (esp. the case with NaOH + water) cooling in an ice bath may be necessary. Remember we're still trying to avoid heat at all costs.
7B-2) While stirring the original acidic solution, slowly add dropwise your basic solution. Stop when you reach pH 11 or 12. This will convert the LSA's back into their freebase form, making them more soluable in non polar solvents. Properly dispose of any unused base, and wash that jar out.
7B-3) Add enough of a low boiling point non-polar solvent (that evaporates cleanly) to your 1st jar to be considered a layer. Put the lid on and shake it for 15-30 minutes.
7B-4) Pour your nearly completed masterpiece into a separatory funnel (pretty cheap on eBay, get Pyrex). Separate the layers. Keep both. Put the polar layer back in the original jar and put the non polar layer in a new, clean glass jar. Make sure to label them, just in case. Repeat the non polar extraction 2 more times to make sure you get all the good stuff.
7B-5) Properly dispose of the now useless polar solution (which will probably contain some dangerous cyanide salts. If the enzyme thing works and NaOH was used was the base then the highly toxic salt NaCN will be present).
7B-6) Combine all the non polar layers. Create another basic solution in another clean glass jar (distilled water and NaOH, household ammonia, or baking soda). Aim for pH 8. After cooling properly, combine the basic polar solution with the non polar in a jar and shake. This is to remove any polar contaminants from the non polar layer. Separate and discard the polar layer. Repeat 2-3 times or more. A slightly basic polar solution is needed so it will not ionize the LSA's making them soluable in polar solutions again.
7B-7) After the polar washes are complete place the non polar solution in a pyrex baking dish and evaporate it. Don't heat it, just place it in an open window or something with a fan blowing across the surface. After the non-polar solvent evaporates, one should be left with some relatively pure LSA extract. The main contaminant would most likely be some fatty plant gunk. The initial non polar wash in step 4 will determine how 'clean' the end product will be.
7B-8) Convert the end product to the tartrate salt as the freebase form is highly unstable.
Both teks need work, and they're mostly just speculation and theorizing.
Comments, additional information or anything else would be kindly appreciated,
One of my primary goals is to determine what chemical(s) present in the seeds cause the ill side-effects commonly associated with their ingestion. So far, I've found that some of the suggested are:
* Essential oils present in the seed pulp that can irritate the GI tract.
* Cyanogenic Glycosides present in the seed coating (similar to the ones in apple seeds) that produce many ill side-effects.
* Pesticide and/or fungicide present on the outside of the seed that may or may not come off with soap and water.
* And finally, the Ergot alkaloids themselves may actually cause many of the ill side-effects everyone wants to avoid.
There are quite a few crude extraction teks online. Most seem to be minimally effective. On another forum, there have been a few new extraction methods suggested:
Method 1:
This tek was suggested to be preformed outside on a cold night due do the use of hexane
Grind seeds into powder.
Place the powder in a glass bottle or flask with a tapered neck that is supported somehow (ring stand or similar).
Spray hexane into the bottle with the seed powder in it.
"it (hexane) is readily available in its purest of forms from any electronic store as an electronic cleaning agent."
Cover the top of the bottle with filter paper and place a rubber band around it to keep it on. Poke a small hole through the middle of it.
Invert the bottle and let the hexane spill into a pyrex baking dish.
The hexane should evaporate very quickly leaving behind a relatively pure extract that's active at ~10mg+.
Method 2
1) Finely grind seeds into a powder. Make sure to maintain a low heat and light environment. Be careful with the electric coffee grinders as the friction creates the heat we're desperately trying to avoid. Using a pepper mill would be a better option (much more physical labor though).
2) Prepare an acidic solution in a clean glass jar. I'd recommend using cold distilled water and a pure, food grade acid (tartaric, acetic, citric, etc). Aim for a pH of around 5. If one were to use a stronger acid, an ice bath may be necessary to keep the solution cool.
3) Put the seeds in the cold, acidic solution. Put the lid on the jar, and shake it for about 15-30 minutes. Any more would be a waste of time IMO.
4) Defat with your non polar solvent of choice (cooking oil is not a good choice). Since what we want is not soluable in non-polar solvents right now, and we're not going to evaporate it away, it's ok to use something like hardware store naptha. Basically this step consists of combining a non-polar solvent with our acidic solution, shaking the two in a jar for a few minutes, separate and discard the non-polar layer, repeat. A separatory funnel is almost required here (they're quite cheap on eBay, get a Pyrex one). The more thourough one is with this step, the less 'gunky' the end product will be.
5) After removing all non-polar solvents from the previous step, we should have the desirables in a more stable form, dissolved in the acidic solution with little if any 'fatty plant crap'. Add a to be determined amount of amylase to the solution. Put the lid on the jar and shake it for however long you think it'd take for the enzyme to do it's thing. Hopefully this will rid our solution of the terrible glycocides.
6) Filter out all seed matter as it is now useless to us.
Now there are two ways we could go from here:
----------------------------------------
7A-1) Heat the solution to 80'F. Stir for an hour or so. This should rid us of the HCN in the solution (I'm not even sure if this will work). It may also rid us of the desirable alkaloids. I really can't say how sensitive the salt forms of the alkaloids are.
7A-2) Drink the solution or store it in the fridge for a later time.
----------------------------------------
7B-1) Another way to go with this (more involved, but may be much more efficient) is to preform a full acid/base extraction. We're now back on step 5 with the filtered acidic solution. In a separate glass jar / beaker create a basic solution. I'd use a 5M NaOH solution in distilled water. Household ammonia and perhaps baking soda would work too. If the creation of the basic solution was exothermic (esp. the case with NaOH + water) cooling in an ice bath may be necessary. Remember we're still trying to avoid heat at all costs.
7B-2) While stirring the original acidic solution, slowly add dropwise your basic solution. Stop when you reach pH 11 or 12. This will convert the LSA's back into their freebase form, making them more soluable in non polar solvents. Properly dispose of any unused base, and wash that jar out.
7B-3) Add enough of a low boiling point non-polar solvent (that evaporates cleanly) to your 1st jar to be considered a layer. Put the lid on and shake it for 15-30 minutes.
7B-4) Pour your nearly completed masterpiece into a separatory funnel (pretty cheap on eBay, get Pyrex). Separate the layers. Keep both. Put the polar layer back in the original jar and put the non polar layer in a new, clean glass jar. Make sure to label them, just in case. Repeat the non polar extraction 2 more times to make sure you get all the good stuff.
7B-5) Properly dispose of the now useless polar solution (which will probably contain some dangerous cyanide salts. If the enzyme thing works and NaOH was used was the base then the highly toxic salt NaCN will be present).
7B-6) Combine all the non polar layers. Create another basic solution in another clean glass jar (distilled water and NaOH, household ammonia, or baking soda). Aim for pH 8. After cooling properly, combine the basic polar solution with the non polar in a jar and shake. This is to remove any polar contaminants from the non polar layer. Separate and discard the polar layer. Repeat 2-3 times or more. A slightly basic polar solution is needed so it will not ionize the LSA's making them soluable in polar solutions again.
7B-7) After the polar washes are complete place the non polar solution in a pyrex baking dish and evaporate it. Don't heat it, just place it in an open window or something with a fan blowing across the surface. After the non-polar solvent evaporates, one should be left with some relatively pure LSA extract. The main contaminant would most likely be some fatty plant gunk. The initial non polar wash in step 4 will determine how 'clean' the end product will be.
7B-8) Convert the end product to the tartrate salt as the freebase form is highly unstable.
Both teks need work, and they're mostly just speculation and theorizing.
Comments, additional information or anything else would be kindly appreciated,
