Experimental Ergoline-Alkaloid Extractions (everything about LSA's)

[Observant]

This thread is all about Full Spectrum Extraction of mainly the Ipomea alkaloids ,as they can have more euphoric ,more visual effects than LSAs from HBWR , due to a unique Alkaloid Makeup.

SWIM is still trying to figure it all out , and he is looking forward to make some practical Experiments... It's a big mystery ....

LA-111, ergine, d-lysergamide. This is an active compound and has been established as a major component in morning glory seeds. It was assayed for human activity, by Albert Hofmann in self-trials back in 1947, well before this was known to be a natural compound. An i.m. administration of a 500 microgram dose led to a tired, dreamy state with an inability to maintain clear thoughts.
After a short period of sleep, the effects were gone and normal baseline was recovered within five hours. Other observers have confirmed this clouding of consciousness leading to sleep. The epimer, inverted at C-8, is isoergine or d-isolysergamide, and is also a component of morning glory seeds. Hofmann tried a 2 milligram dose of this amide, and as with ergine, he experienced nothing but tiredness, apathy, and a feeling of emptiness.

Both compounds are probably correctly dismissed as not being a contributor to the action of these seeds.
It is important to note that ergine, as well as lysergic acid itself, is listed as a Schedule III drug in the Controlled Substances Act, as a depressant. This is, in all probability, a stratagem to control them as logical precursors to LSD.

The average morning glory seeds according to samples tested in 4 different parts of the world contain 29.75 milligrams of alkaloids on average per 100 grams of seeds.

Now per gram that breaks down into 0.2975 milligrams of alkaloids per gram of seeds.That is 297.5 micrograms of alkaloids per gram.

A common and moderate dose of morning glory seeds is 100 seeds.That is roughly 3.4 grams as the average seed weighed approx 34 milligrams each.

Now seeing as on average each gram of seeds contains 297.5 micrograms of alkaloids that means 3.4 grams of seeds contains 1,101.5 micrograms of alkaloids.

Science says LSA is one tenth as potent as LSD.This means that 3.4 grams of seeds would be equivalent to 101.15 micrograms of LSD.That is just barely over one hit of LSD as one hit of LSD is 100 micrograms.Research seems to support this formula.

Now if you take 100 seeds(the dose) and divide that by 1,101.5 micrograms of alkaloids it comes to 11.015 micrograms of alkaloids per morning glory seed.That is the equivalent of 1.1015 micrograms of LSD per morning glory seed assuming the seeds contain the average 29.75 milligrams of alkaloids per 100 grams of seeds.

However seeds analyzed ranged from 10 milligrams of alkaloid per 100 grams of seeds in the worst case and 52 milligrams of alkaloids per 100 grams of seeds.

This means that 100 morning glory seeds can range from 340 micrograms of alkaloids per 3.4 grams (or approx 100 seeds) to 1,768 micrograms per 3.4 grams (or roughly 100 seeds).That means in the lowest sample analyzed (10 milligrams of alkaloids per 100 grams of seeds) would be equivalent to only 34 micrograms of LSD (or approx 1/3 hit)while the highest sample analyzed (52 milligrams of alkaloids per 100 grams of seeds) would be equivalent to 176.8 micrograms of LSD (or approx 1 and 3/4 hits).

In conclusion one can expect the average morning glory seeds to contain the equivalent of 101.15 microgams LSD per 100 seeds but it can range from the equivalent of 34 micrograms of LSD to the equivalent of 176.8 micrograms of LSD per 100 morning glory seeds.

On a per seed basis the average sed contains is the equivalent of 1.1015 micrograms of LSD but can range from the equivalent of 0.34 micrograms of LSD per seed to the equivalent of 1.76 micrograms of LSD per seed.

LSD is an unusually fragile molecule and some comments are in order as to its stability and storage. As a salt, in water, cold, and free from air and light exposure, it is stable indefinitely. There are two sensitive aspects of its structure.

The position of the carboxamide attachment, the 8-position, is affected by basic, or high pH, conditions. Through a process called epimerization, this position can scramble, producing isolysergic acid diethylamide, or iso-LSD. This product is biologically inactive, and represents a loss of a proportionate amount of active product.

A second and separate point of instability is the double bond that lies between this 8-position and the aromatic ring. Water or alcohol can add to this site, especially in the presence of light (sunlight with its ultraviolet energy is notoriously bad) to form a product that has been called lumi-LSD, which is totally inactive in man.

Oh yes, and often overlooked, there may be only an infinitesimal amount of chlorine in treated tap water, but then there is only an infinitesimal amount of LSD in a typical LSD solution. And since chlorine will destroy LSD on contact, the dissolving of LSD in tap water is not appropriate.

Some LSA Related Web Sources I recommend :

https://dmt-nexus.me/Files/Books/General/LSA%20Extraction.pdf

"1975 paper detailing 3 methods of alkaloid extraction from morning glory seeds."

https://kb.osu.edu/dspace/bitstream/1811/22310/1/V075N4_198.pdf

Erowid LSA Vault: Erowid LSA Vault
Ergine : Ergine - Wikipedia
LSH : Lysergic acid hydroxyethylamide - Wikipedia

Erowid Experience Report on Ergine Extraction : Morning Glory - Erowid Exp - 'Ergine Extraction'
Pictorial on Mycotopia : http://forums.mycotopia.net/botanic...62848-lsa-extraction-morning-glory-seeds.html
Psychedelic Chemistry Book - LSD Chapter : Psychedelic Chemistry - LSD
The Original 11 Pages Thread where the Experimental extraction came up : http://www.zoklet.net/bbs/showthread.php?t=14328
Peter Webster : Mixing the Kykeon.pdf - http://www.erowid.org/chemicals/lsa/lsa_article1.pdf
More Kykeon Chemistry : Ibogaine Protocol Submitted to IRB - Multidisciplinary Association for Psychedelic Studies - MAPS
Giantic Shroomery Thread : Giganthum Morning Glory extracts & experiences thread - The Ethnobotanical Garden - Shroomery Message Board

Shulgins Tihkal : LSD-25 +Morning Glory Entry : http://www.erowid.org/library/books_online/tihkal/tihkal26.shtml
Albert Hofmann : Ergot , Rich Source of Pharmacological Active Substances ( Great! ) : http://www.lycaeum.org/research/researchpdfs/2343.pdf
Another good Document by Hofmann : http://www.erowid.org/plants/mushrooms/references/other/1971_hofmann_bulletin-narcotics.shtml#s200

Biotech Eyecandy : http://www.erowid.org/archive/rhodium/chemistry/articles/claviceps.paspali.html
Shroomery about the above : http://www.shroomery.org/forums/showflat.php/Number/7018848
Claviceps Identification : http://www.erowid.org/archive/rhodium/pdf/claviceps.identification.pdf

No PhD required : http://forums.mycotopia.net/misc-entheogens/9372-peptide-coupler-method-lsd-production.html
http://www.mediafire.com/?lznmdmkok0z - The Alkaloidal constituents of hawaiian baby wood rose, argyreia nervosa PDF
http://www.lycaeum.org/research/index.rbx?id=4941 - Chromatographic separation of iysergic acid amide and isolysergic acid
amide in Morning Glory seeds

Ipomea Violacea grows up to over 8metres in height !

 

[Observant]

thread is long and informative

http://www.zoklet.net/bbs/showthread.php?t=14328&page=7

First off, this is still in an experimental phase, so I don't suggest that anyone here try this without at least reading the entire thread. Even if you do read it, I can't guarantee results.

Experimental extraction

Quote:

1. Get crapload of distilled water from store. Not mineral water, distilled. Let stand overnight then put it through a water filter anyway, just in case they lied and poured it from the tap.

2. Using your usual volume per amount of seeds, mix up a batch of bicarbonate solution (baking soda + distilled water). Soak the seeds overnight, pouring through a coffee filter to catch any undissolved baking soda.

3. Repeat step 2.

4. Soak the seeds for 1-2 days in ordinary (baking-soda-free) distilled water, for a nice CWE. Or at least a water extraction. Add 1-2 capfuls of vinegar (or your desired amount of tartaric acid) for luck.

5. Pour off water through coffee filter into an empty container.

6. GENTLY add little sprinkles of baking soda until it stops foaming... at which time you can just start adding teaspoons at a time until little white rocks form. If you're using a container you can close and shake, this would be a good thing...

7. Pour through coffee filter.

8. Make dilute bicarb solution by pouring baking soda into distilled water and then pouring off through a filter paper as before... then, add twice its volume in distilled water.

9. Pour a few splashes of the dilute solution through your coffee filter in the funnel until the bicarb stops rinsing away, and only the little white rocks remain.

10. Shake the little white rocks out on a mirror or glass table, which has been cleaned of dust beforehand. Do NOT eat them all at once, lol.

11. Scrape little white rocks and powder from the mirror into a clean cap from a 2l bottle. Fill a dropper bottle (visine, candy drops, etc) with distilled water - a few sprinkles of vitamin C help here, if you've got 'em - and squirt it out into the bottlecap. Sprinkle in tartaric acid until the little white rocks dissolve, and suck them into the vial.

12. Try a few drops. If that doesn't work, wait a week for your tolerance to go down and try a few more drops. If you've got a good milligram scale, you can actually do this in mg/drop, but otherwise, you'll just have to make up your dose as you go along from an educated guess.

Congrats on your vial, dude.




(and yes, heat, you should be able to chuck the little white rocks into some H2SO4. Of course, you can just precipitate the LA straight from tea, too, via filtering and subsequent overacidification).

Oh. It helps to do this from a LOT of source stock (2oz+), because finding a five milligram speck to catch it is sometimes kinda hard. Better to have 15 and 20mg rocks forming a lot more milligrams in a pile. Plus, it works better to have more than one dose in a hundred-drop vial, lol.

1. 112g of ipomea tricolor, var. heavenly blue, were pulverized and placed into a large, clean plastic container.

2. 4 fl. Ozs of 5% acetic acid solution was added.

3. Distilled water was added to between 4x and 8x the volume of seed mass.

4. The solution was allowed to sit, in the dark and refridgerated, for 2-6 weeks.

5. A giant-ass cottonball was jammed into a 3l plastic funnel, and the solution was slowly filtered over the course of up to a few days, possibly repeatedly until the suspension is clarified, yielding...

IPOMEA TEA!!!

6a. Sodium bicarbonate was added, with stirring, at a rate of approx 10mg/s over the course of several hours... OR...

6b. With much laziness, aqueous ammonia was added at 1 drop/second....

...until about 2x the volume present upon the first instance of precipitate is added, OR (in the case of bicarb) until the bicarbonate no longer dissolves.

7. The solution is let stand in the dark, UNDER REFRIDGERATION, for anywhere from 4-24 hours.

8. A small plastic funnel is selected, and a coffee filter placed over the outlet tip, secured with a rubber band 1cm up the stem.

9. A second, larger funnel is outfitted with a coffee filter internal to the funnel. This is used to catch the outlet from the smaller funnel.

10. The basified solution is decanted through the small filter, whose outlet pours into the larger filter. A wide jar with a narrow mouth is ideal here, as it allows you to 'flip' the alkaloidal sediment out and rinse it down without heavily pressurizing the filtration point.

11. Some of the wastewater is tossed back in the jar, swished around a tad, and poured into the small funnel to go through the entire filtration setup.

12. A 5ml wash of aqueous ammonia is sent "down the hatch," gently.

13. The coffee filters are detatched and allowed to dry in the dark next to a container of MgSO4 in CO2 atmosphere under refridgeration.

14. The bulk of the alkaloids withdrawn from the filter on the small funnel and neatly tipped out of the "cup" formed by the placement of the rubber band, where they should form a small pile. Flicking the tip of the "cup" while it is upside down should dislodge small piles of trace dust.

15. 20 drops of citric acid solution are added, and a drop is placed on the tongue.

16. A report is posted on F&B, for great justice...

16b. If this was not effective, proper procedure (in order) is to...

- drink the waste water (which was in the fridge, amirite?)

- eat the seed pulp. See if you trip while puking your guts out.

- drink lemonade out of the basing jar. See if you stuck it all on the sides. And...

- eat the filter papers. See if the dust is still trapped.

If none of those four turned up anything, there were no psychoactives in your seeds, lol.

...for those who were wondering, the slow-ass basification is all about encouraging the increase in conglomeration size. Coffee filters are much more effective at catching a 30mg rock, two 20mg rocks, and five 10mg rocks than they are at catching 10,000 10ug specks.

No one (except harry) knows if this will work... but after eating the "magic four," we'll sure as hell find out where it ended up, won't we?

 

[Phlux-]

i posted this exact post a few days ago - also pasted from mycotopia - check - some tek i found (lsa) - LSD, LSA, LSH - Welcome to the DMT-Nexus
duplicate post.

 

[Observant]

oops , didnt see that one ... cant believe nobody replied on this .
The Guy who originally posted his tek also stated that he successfully extracts from all plant parts of Morning Glories.

I definitely want to try his method , but i am also quite anxious it won't work .

The Kykeon Article by Peter Webster can be found in this Journal : http://earthrites.org/invisible-college/IC-Beltane07sm.pdf
Very very Informative 10 pages , ( Pages 24-34 ).



Here is some more Information on the Alkaloidal Contents of Morning Glory Vines . We're not just talking about one compound

Below is a list of LSA contents in morning glory, and misc. other seeds and
plants.

***************************************************************************
LAA% Total Alks. % by weight

Hawaiian baby wood rose: 0.04 0.30
Ololiuqui: 0.02 0.04
Heavenly Blue: 0.01 0.02
Pearly Gates: 0.02 0.03
Wedding Bells: 0.01 0.03

Taken from :
Isolation and Identification of Lysergic Acid Amide and Isolysergic Acid
Amide as the Principal Ergoline Alkaloids in _Argyreia nervosa_, a tropical
wood rose. Michael D. Miller (Bureau of Narcotics and Dangerous Drugs . Journal of the AOAC, vol 53(1):123-7, 1970.


***************************************************************************
Major Alkaloid Content in the seeds of A. nervosa(Burm. f.) Bojer

[snip] % of Total alkaloid % dry seed weight
Ergine 22.68 0.136
Isoergine 31.36 0.188
Ergometrine 8.20 0.049
Lys. alpha-OH-ethylamide 5.79 0.035
IsoLys. || 3.98 0.024

Taken from:
Ergoline Alkaloidal Constituents of Hawaiian Baby Wood Rose, _Argyreia
nervosa_ (Burm. f.) Bojer. Jew-Ming Chao and Ara H. Der Marderosian.
Journal of Pharmaceutical Sciences 62(4):588-91. 1973.

All these alkaloids listed here can be hydrolysed into Lysergic Acid.
This will also racemate it, but so what, according to this chart
the iso form is more predominant anyway, racemization should thus
produce more of the biol. active form. Also, isolation of the iso form
(chromatography) followed by racemization will give still more active stuff,
but probably not worth the trouble.

found here : http://www.maps.org/old_forum/1999/msg00844.html

Just want to post up the ergoline alkoloid content of containing seeds for your guys benifit.

As taken from Otto Snow's "LSD-25 and Tryptamine synthesis"

Rivea Corymbosa(Ololiuqui)

.021%-.060%

Ipomoea Violacea(Morning Glory)

.005%-.079%

Argyreia Nervosa(HBWR)

.5%-.9%

The seeds are approximately 1 gram / 30 seeds. I seriously don't recommend going above 15 grams (450 seeds). 7 grams is alright for a test dose. Physical side effects can be unpleasant (I get vasoconstriction and notice that my hands feel cramped).


Lysergic acid amide itself (ergine) one of the ergot alkaloids found in morning glory seeds, but IIRC Hofmann thought ergometrine (ergonovine, lysergic acid propanolamide) may be the principle psychedelic.

* Ergine (Lysergic Acid Amide, LAA, LA-111, Lysergamide)
* Isoergine (Isolysergic Acid Amide)
* Ergonovine (Lysergic Acid Propanolamide)

The chemicals found in much lower concentrations are:

Agroclavine
Setoclavine
Restuclavine
Cycloclavine
Lysergine
* Elymoclavine
* Lysergol
Penniclavine
Chanoclavine


* - indicates that the substance is thought to have psychedelic activity.

And Some thread from Edot : entheogen.com

 

[Observant]

Maybe... if you have access to DCM and a Soxhlet :

I got some cooky idea's. Lets have a look at em.

You could extract the LSA using this method. It involved a sohxlet so it is mostly automated.

SWIM does a special LSA specific double A/B extraction on the seeds. That effectively gets rid of the toxins. If you can extract DMT, you can extract LSA, but it’s a slightly different process.

You extract with boiling acetone. Evaporate that, then dissolve in water and you do 8 defats with DCM to get rid of most of the toxins.

You then freebase at pH 9 with sodium carbonate. Then during the freebase stage you cannot do any water washes or you’ll lose product (just like with mescaline). You extract 5 times with DCM. Then distill off most of the DCM, until down to about 25 ml.

Then extract with dilute hydrochloric acid or vinegar. Then defat again about 3 times with DCM.

Then freebase at pH 9 and extract with DCM 5 times. Then distill off most of the DCM, until down to about 25 ml and let the rest evaporate to get fairly pure freebase LSA and some other alkaloids.

Then the Lysergic acid and it amides could be further purified using this column chromatography method

http://research.lycaeum.org/index.rbx?id=4941

Turn the Lysergic acid amide into Lysergic acid pyrazole then into lysergic acid diethylamide using the following proceedure

Proceed directly from the amide to LSD: Treat the amide or amides with anhydrous hydrazine to form the hydrazide, followed by actylacetone to forn lysergic acid pyrazole, which forms LSD on treatment with diethylamine

And once again use column chromatography to purify the final product then turn into a tartate salt.

That's just a rough outline, and through all my research seems to be the best way to moved from morning glories to LSD. If anyone see's any glaring problem with this, just say so.

Been a while since I have been around. It seems like the ergoline alkoloids present in morning glories, Rivea Corymbosa, and Argyreia Nervosa seem to be resistant to heat. Or at least the important ones seem to be. The tek that I posted was not developed by me, it was developed by a chemist. I will state right now that I am not a chemist. Otto Snow is a chemist on the other hand, and I will post and excerpt out of his book, "LSD-25 and Tryptamine synthesis."

"Pulverised seeds (100 grams) must be defatted before extraction of alkoloids. Naptha or petroleum ether are suitable solvent for fat extraction of the seeds. The seeds can be refluxed in the solvent or they can be reflux in a sohxlet extractor. The seeds mash is then filtered from the solvent. Total extraction of the fats is present when new solvent extract leaves no greasy residue on evaporation.

The seed mush is then allowed to dry of solvent, mixed with 500ml of 10% ammonium hydroxide (storng ammonia water) and extracted with ether or appropriate solvent. Evaporation of the solvent leaves the alkoloids."

That is from page 33. Looks like there is not much to worry about when using a hot solvent extraction. If there is an alkoloid loss it is probably very minimal.

And for those of you who are still concerned about heat, you could do the defat under vacuum and use DCM as the solvent. That is presupposing that the extract will be used in some kind of diethylamination. So you should have vacuum equipment already. The boiling point of DCM should fall below 29* Celcius at around 400 torr. DCM could also be used in the extraction and evaporation phase.

 

[Observant]

Words of Advice from the Nexus Member "69ron" :

SWIM's first crude LSA extraction used isopropyl alcohol and it was highly successful.

You can extract LSA from the seeds using the following solvents that SWIM tested:

Water
Isopropyl Alcohol
Ethyl Alcohol
Acetone
Methyl Ethyl Ketone

You can NOT extract LSA from the seeds using these solvents:

Naphtha (that includes V&P Naphtha, charcoal lighter fluid, etc.)
DCM (Dichloromethane)
Xylene
Heptane
Toulene



The LSA is present in the seeds in water soluble salt form. When in freebase form it is soluble in the following solvents that SWIM tests:

Water
Isopropyl Alcohol
Ethyl Alcohol
Acetone
Methyl Ethyl Ketone
DCM


The best way to extract LSA is by using an A/B extraction. In order to do an A/B extraction on it, you must use DCM or a similar solvent as the NP solvent. Water soluble salt forms of LSA are insoluble in DCM. But freebase LSA is soluble in DCM and water. When in the A stage, you should defat about 10 times with DCM to ensure all the toxins are removed. Then go to the B stage. Note that, in the B stage the freebase form of LSA is still soluble in water. So in the B stage, you need to extract the freebase LSA from the basic water at least 10 times using DCM. But when going from DCM to acidic water, 1 time is usually enough because it LOVES WATER. You’ll want to go from A to B and then back to A again. The reason being that freebase LSA is very unstable, so after you freebase it, you’ll want to immediately convert it back into a salt. LSA is colorless but fluoresces in black light. It’s very helpful to have a black light. This helps you tell if all the LSA is extracted or not. During the B stage, the DCM will glow in black light if there’s any LSA in it.

Note that you should not boil LSA for very long or it will eventually decompose. So if you want to extract the seeds using a Soxhlet, use a low boiling solvent like acetone.

The alkaloid extraction was done in a 1000 ml Soxhlet using 600 ml of acetone. 23 grams of coarsely ground Argyreia nervosa seeds (102 seeds) were put into a glass extraction thimble placed in the Soxhlet. The acetone was boiled and cycled through the Soxhlet for 3 1/2 hours for a total of 11 siphons (i.e., 11 automatic extractions with boiling hot acetone).

Next, the acetone was distilled down 50 ml, and then 100 ml of water was added to it.

The pH of the solution was measured and found to be around 5. The pH is adjusted to 3 with citric acid.

The solution is defatted 8 times with 50 ml DCM. The solutions can be shaken vigorously without an emulsion forming. The first defat produces a light tan water layer and an amber DCM layer. By the 4th defat both layers are colorless. We do 8 defats to be sure all the toxins are removed.

Next we adjust the pH to 9 with sodium carbonate. The water layer is extracted with 50 ml DCM 5 times.

Next we distill the DCM with the freebase LSA (and other alkaloids) in it. We distill down to 50 ml and then evaporate the rest of the DCM in a shallow pan. The extract becomes light tannish yellow and it evaporates away. Once dry it amounts to 72 mg (about a 0.3 % yield).

At this point the extract is probably 90% pure alkaloids, most of which is freebase LSA. It's impure, tannish yellow and slightly sticky but extremely potent.

You'll want to make a salt out of it. LSA tartrate is recommended.

There are several cleanup steps that can be done, but all seem to greatly diminish yields. So I'm not sure if they're really worth it.

SWIM's is extracted and purified white LSA tartrate crystals. He had help from a friend who isolated the LSA from the other alkaloids, but he did the alkaloid extraction himself. He made a glycerin tincture out of it with vitamin C added as an antioxidant. It's been kept at room temperature in an amber bottle for over 2 years now and still works very well.

SWIM got it from a book. Basically do a standard A/B extraction, but use a semi non-polar solvent like dichloromethane, ether, or chloroform. Non-polar solvents like naphtha or heptane don’t work.

After extracting into pH 3-4 water, you’ll need to do many defats using dichloromethane (or ether, or chloroform, whichever solvent you decide to use for the freebase extraction). We’re talking at least 10 defats.

When freebasing LSA, you want a pH of 8.5-9 and don’t bring the pH above 9 because LSA can be destroyed. Then extract the LSA from the water 10 times using a solvent like dichloromethane. 3-5 times is NOT enough. Don’t do any water washes of the dichloromethane. Freebase LSA is very water soluble. When in freebase form, water washes will extract it from the non-polar solvent even if the pH is very high. So don’t do it.

Next extract into water 3 times using pH 3 water. Defat again at least 10 times. Freebase again at pH 8.5-9. Extract 10 times into dichloromethane, distill off the dichloromethane (or evaporate it). This leaves behind pure white freebase LSA crystals. They should be converted to a salt at this point. This can be done by dissolving the crystals in a tiny amount of 10% hydrochloric acid at pH 3-4 and letting it all evaporate.

SWIM only did this extraction one time. So he’s not an expert at all on this particular extraction, but he understands what all the steps are for.

The soaking time should be overnight for best results.

You can use IPA instead of everclear.

You definitely want the alcohol step. It helps to get a more pure end product.

No one knows exactly what in the seeds cause which side effects. This extraction process is fairly good and does remove some of the toxins. The oils in the seeds are said to be very irritating to the stomach and washing with a non-polar solvent like lighter fluid, naphtha, heptane etc., removes these oils.

You can get a cleaner end product if you dissolve the final product in acetone, and then filter, and evaporate the acetone. LSA is very soluble in acetone. Then take the end result of that, and dissolve it in water, filter, and then evaporate the water in a food dehydrator set on low (115 F or so). What these extra steps do is to remove alkaloids that are insoluble in water and insoluble in acetone. The LSA in the seeds is soluble in water, acetone, IPA, methanol and ethanol, and insoluble in non-polar solvents like lighter fluid, naphtha, heptane, etc.

The end results are very potent and quite dangerous and should be diluted in something like edible ethanol or a water:glycerin mix to both dilute it and preserve it. The mint extract sold at the supermarket is about 90% ethanol and also contains peppermint oil, which might be good for making LSH out of your LSA (SWIM uses peppermint tea for LSH conversion, but this might also work well).

 

[Observant]

a hiver helped me out and provided me a procedure something like this, i tried it on smallscale, never filtered. the results were as expected

extract the seeds with some acetone, add some NH3 solution dropwise, small clouds of LSA will precipitate. the amount is so small that youre going ot need a centerfuge or at least to ahve to wait a while for it to settle. then you can suck off or decant most of the acetone and filter the solution, i think useing printer paper would be the best choice. patence is key. then it would be good to add a few grains of citric or tartaric acid to make it last longer.

 

[damiana]

your truly on to something here, I hope you figure it out. A few test runs would help, if someone has the time and the supplies.

 

[Observant]

:lol:

I'm pretty sure the violacea produces ergoloids itself, but this has... other interesting implications.

Posted on, I think the Hive, once upon a time, was a fascinating little find - that claviceps purpea is actually capable of producing LSD if fed ipomea-produced lysergic acid ethylamide - that purpea and violacea ethylation enzymes not only target different hydrogen, but are not blocked by prior ethylation...

...so if a dicot-substrative claviceps exists, known to produce ergoloid alkaloids exists, and if its metabolism is enzymatically identical to the monocotymous purpea...

...LSD-seeds straight from the plant might be a possibility

biosynthetic acid
Posted 02 August 2010 - 05:21 PM

Quote
Method X is VERY secretly distributed..but takes a little (lot) of research to figure out the golden reference (somewhere) in royal society of (...??) describes a method to biosynthesize the great acid by "tricking" claviceps paspali in to producing it by modifiying the growth substrate to produce strictly the d- stereoisomer therefore bypassing synthesis or starting materials. Grow it on the "special, modified" subtrate...extract the goods...chromatograph for the purity freaks...and enjoy. This so called product is called "the natural" and boy oh boy. Wowee... Dont ya love how nature can synthesize stuff for ya! Amazing. Thats all I can say..Please dont email me regarding the refs/info. As I have none. Thats not my bag baby! Pays to know certain people I guess. Enjoy the search...takes a year or so to find the specifics. BTW- DEA hates this shit..amateurs need not apply. Leave this one to the pros. Enjoy!


that is just a random post I found on SM somewhere. But, even though it is vague...does that have even the slightest chance of being true?


Quote
Im not trying to be a cryptic know-it-all here. But- ever wonder why no one talks about making the stuff...and every internet "recipe" out there is so detailed and outdated that anyone who even attempts it would be taking on a huge investment, requiring elaborate lab equipment, and more importantly- starting materials that the DeEeAy has long since flagged for decades. If a person is smart- they wouldnt even touch it with a 10-foot pole. It is distributed online strictly as a novelty. Did the hippies in the 60's and 70's do it this way?- When they came to parties with gallon jugs of the stuff?? I think not. Using a reference database these days like scifinder scholar turns up hundreds of different juicy tidbits on circumventing these "perceived" hurdles- one bypassing another to get an end result. People who actually do, do it..are really, truly on a quest for the correct (current) information for a viable method of clandestine production- not Hoffman's original synth of step by step, tedious labwork from materials that were handed down to him. And, when they do actually find it--they are not so quick to just give the info away. I did have one journal reference that I found after a long search of everything that was out there in college libraries, chem journals, alt. knowledge books, etc. And when I did finally find this- and read it- a big bright light flicked on in me..and a huge grin took over my face. I did not even want to attempt what was in the text. Having the knowledge was sufficient enough. And that is why the info isn't just "given out"--its the journey, not the destination. All I can say is- start with claviceps paspali when you begin the search...



From Another poster:

Quote
I found something about the Proceedings of the Royal Society of London in US patent 3224945. Also see US3219545

 

[Observant]

right on, well then the post came from a member of the hive (https://www.the-hive.ws) who went by the screen name halfapint. The original post was from 07-12-00 and I'll post it and some other posts from the thread which are informative that were made by halfapint. I'll list the date of the post before each post to kind of seperate them.

07-12-00

Morning Glory Whole Plant Extract

Who says submerged culture of Claviceps is preferable to exploiting profuse native morning glories to get lysergic goodies?

SWIM wanted to check the morning glories of her native environment, on a hunch. The hunch came from persistent reports of allergy / toxicity at the touch of morning glory foliage, in Mesoamerica and in North America. Large effects from trace amounts is a lysergic specialty, and mg's don't have a bunch of other bad alkaloids in them. Everybody says morning glory seeds only, and then just from certain varieties.

So thinking such thoughts, SWIM hopped out and gathered up a bunch of wild plants, genus ipomoea. She performed extraction procedures on the first 4 spp. of wild or feral mg's she found, with 2 domestic varieties, blue and purple, for comparison.

So SWIM extracted in this wise: the air-dried plant material was macerated, then moistened with 0.1 N sodium carbonate aq. to free the base. The material was percolated in a column with 1 liter petroleum ether added dropwise over 6 hours. Dilute acid, SWIM said 0.02 N HCl, was used to extract the hopeful-amide from the nonpolar solvent, in three vigorous washings (200, 200, 100 ml) in a 2-liter bottle. Coincidentally, that same bottle was used as separatory funnel, by inverting it and carefully loosening the cap.

But that ain't the point. The point is, that SWIM worked under black light all she could, to see what was going on. She saw florescence in the layers, giving visual feedback on the progress of the separations. The more concentrated the alkaloid, the brighter it glowed, typical of the indole ring alkaloids. In this case, SWIM figured glow meant LAA, lysergic acid amide, because morning glories don't have any appreciable amounts of any other lysergic acid derivatives, nor any other indole alkaloids, nor any other alkaloids at all.

So after the brightly-glowing aqueous fraction was cut out, SWIM made the solution basic with ammonia, giving a flocculent precipitate which took forever to settle out. But it glowed.

SWIM did this on all 6 plant materials, and the situation was the same with all the extracts of morning glory whole plants. Making the same type extraction on crushed domestic seeds did produce a greater concentration of product, as might be expected.

But I says to Swim, I says look. The respectable books and sources and stuff all say it ain't true, you can't get lysergic stuff except from the seeds, and just certain kinds of seeds, and better you just go score Hawaiin Wood Rose and forget plain old morning glories, but you just proved them wrong. Six times out of six tries, you got glowing alkaloids from the leaves, and vines, and stems, and tendrils, and seed cases, and stuff like that all mixed together. So is somebody trying to hide something, or did you just get lucky?

SWIM says, well fuck that, the real reason to use morning glories is because there's only one compound worth worrying about, but if you use ergot you need to fool with seventeen different types of ergotosnotalines.

Well this is a cliff hanger, and SWIM isn't real happy about using ammonia because it makes the ppt. way too puffy and hard to filter for the next stage, but she just persisted with the same technique so all the batches would be treated the same, so she could compare them.
Next time I spot her, I'll ask her how it's going.

07-13-00

The amount of plant material was ~100 grams in each case, perhaps a bit less because this was dry weight and herbaceous materials lose a lot of weight when they dry. Yes there were differences between the species, but as I mentioned I don't expect to provide this particular bit of documentation.


The last reference I have refers to isolation of ergot alkaloids from Ipomoea violoacea:

Moekatis et al, Biochem. Physiol. Pflanzen, 1973, 164, 248.

Seeds:
-pulverized seeds defatted in pet. ether for 5 hrs.
-1 g of this material shaken 3X (each for 1 hr.) w/ 20mL of (2g tartaric acid in 30 mL H2O, 70 mL acetone) mix
-combined extracts heated on H2O bath (55?C) to expell acetone
-tartaric acid soln. shaken 3X w/ anhydrous ether, then basified (pH 8-9) w/ NH4OH
-from this soln' alks extracted 3X w/ 10 mL DCM
-combined extracts reduced to 1 mL and chromatographed

Roots, Leaves, Stems:

-pulverized material (15g) wetted w/ 3% NH4OH
-extracted w/ 200 mL DCM in Soxhlet for 6 hrs
-condensed to 20 mL & shaken 4X each w/ 10mL 2% tartaric acid
-total of 40 mL soln. extracted 3X each w/ 10mL anhydrous ether
-tartaric acid extract made basic w/ NH4OH (pH 8-9) & shaken 3X w/ 10 mL DCM
-total of 30 mL DCM extract condensed to 0.3 mL & chromatographed...




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

so there. I know, there's no results of a quant. nature in this brief excerpt, even as I gave no quantities, but the point is qualitative. There are ergotogoodies in m.g. vegetation, and in my experience that is the rule and not the exception.

Otherwise, why would the working pros who did this real published chemistry have bothered to mention extracting from the vegetation, in their peer-reviewed paper? They might have got a wild notion, like SWIM did, and done the legwork, like SWIM did, but if they got zero yields (unlike SWIM), they likely as not would have quietly let it drop when it came time for the writeup.

I haven't seen their paper and don't know their results. But by my guesses into scientist behavior, my bet would go that they found alkaloids also. No point in chromotagraphing 0.3 ml of nothing...

 

[Observant]

Alkaloid Extraction (short method)

Finely grind seeds (preferably woodrose) and add NaHCO3. Extract with ethyl acetate by soaking about one day. Filter and extract the ethyl acetate with tartaric acid solution. Basify the extract with NaHCO3 and extract it with ethyl acetate. Dry and evaporate in vacuum the ethyl acetate to get the alkaloids. Repeat this procedure on the seeds until no more residue is obtained.

Alternatively, add 100 ml petroleum ether to 100 g finely ground seeds and let soak about two days. Filter, discard petroleum ether and let seeds dry. Add 100 ml methanol to the seeds and let soak about two days. Filter, repeat extraction with another 100 ml methanol and evaporate in vacuum the combined methanol extracts. The residual yellow oil contains the alkaloids.

For chromatographic purification of ergot alkaloids from seed extracts see Phytochem. 11,1479( 1972). For ergot extraction and separation see also Fr. Patent 2,089,081 (11 Feb 1972) and CA 79,105,457(1973). For a recent review of the ergot alkaloids see R. Manske (Ed.) The Alkaloids, vol. 15: 1-40(1975).

Extraction of Lysergic Acid Amides from Woodrose Seeds or Powdered Ergot

Reduce the seed material to a fine powder in a blender, and spread it out to dry. Grind it again if it is not fine enough after the first time due to dampness. Saturate the powdered seed material with lighter fluid, naphtha or ligroine. When completely saturated, it should have the consistency of soup. Pour it in a chromatography column and let it sit overnight. Remove the fatty oils from the material by dripping the lighter fluid or other solvent through the column slowly and keep testing the liquid that comes through for fats by evaporating a drop on clean glass until it leaves no greasy film. It will take several ounces of solvent for each ounce of seeds. Mix 9 volumes of chloroform with 1 volume of concentrated ammonium hydroxide and shake it in a separatory funnel. When it settles the chloroform layer will be on the bottom. Drain off the chloroform layer. Discard the top layer. Drip the chloroform wash through the column and save the extract. Test continuously by evaporating a drop on clean glass until it ceases to fluoresce under a black light. Evaporate the chloroform extracts and dissolve the residue in the minimum amount of a 3% tartaric acid solution. If all the residue doesn't dissolve, place it into suspension by shaking vigorously. Transfer the solution to a separatory funnel and wash the other vessel with acid in order to get all the alkaloid out. Pour the washings in the funnel also. Basify by adding sodium bicarbonate solution, and add an equal volume of chloroform. Shake this thoroughly, let it settle, remove the bottom layer and set it aside. Once again, add an equal portion of chloroform, shake, let it settle and remove the bottom layer. Combine the chloroform extracts (bottom layers) and evaporate to get the amides.

Legal Acid

I want to emphasize that "legal acid" can be obtained if other amines are substituted for diethylamine in LSD synthesis. These other lysergamides should give identical trips, but most of them are less potent than LSD. Precise potency data do not exist, so it remains for an enterprising chemist to gain immortality by adding each of the following amines (and any others that come to mind) to separate aliquots of the final step of LSD synthesis (they could easily be done simultaneously), isolating the tartrates and assaying them for potency: piperidine, diisopropylamine, ethylisopropylamine, ethylpropylamine, methylethylamine, methylisopropylamine, tetrahydrooxythiazine, tetrahydroisoxazine, dioxazole, 2-methylmorpholine, 2,5-dimethyl (or dimethoxy) pyrrolidine, cyclo-butyl-amine, cyclopentylamine, etc. Published potency data expressed as a fraction of LSD activity follow: pyrrolidide (1/20), dimethylamide (1/20), morpholide (1/10 or 1/3), ethylpropyl (1/3), dipropyl (1/10), methylethyl (less than 1/10), methylpropyl (less than 1/10).

all quotes taken From : Erowid Search Results for claviceps

 

[1992]

This thread is awesome. Also if the morning glory as the same metabolic pathway as ergot fungus then I know what to do!

 

[Observant]

Thanks! What is it you are thinking of ?

 

[Darkbb]

So does ron's method have a high success rates?? If we get some reports I think it would be a good idea to make a sticky for easy access. I read through the 11page thread and the method changed almost every half page leaving me kinda confused. This is why I like sticking around here at the nexus. I think we do a good job on organizing our methods : ) peace

 

[damiana]

1. Make a paste by mixing the Powdered Seeds with Sodium Bicarbonate.
2.Let the Paste dry completely
3.Extract with anhydrous Isopropyl Alcohol
4.Let the Isopropyl Alcohol Evaporate completely in Evaporation Dish
5.Redissolve in measured Acidic high proof Ethanol (possibly with Peppermint Extract)

When swim gets some time in about two weeks he is going to try and do this. For now he wants to look more into what base and acid would work best with this tek. Why sodium bicarbonate? Is that the best choice? Also what salt is lsa stable in the most? Which acid is the best but still easy to get a hold of? These I will post when I learn, if anyone else knows please add. Thanks.

Damiana

 

[Observant]

I think the best Acids would be Tartaric Acid and Citric Acid - I dont know about Fumaric Acid.
The most stable Form of LSA is said to be the tartrate-salt.

As base i would pick the not so strong ones , like Sodium Bicarbonate or Sodium Carbonate

Be sure to use distilled Water - Chlorine is said to destroy LSA and LSD.

The Chems for this Extraction are all easily obtainable.

Cant wait for the Seed Harvest ...

Good Luck

 

[damiana]

Wow that saved me some time. thanks. SWIM will use sodium carbonate and if he can get a hold of tartaric acid he'll use that. Also what you said above makes me realize why some teks for cold water extraction using peppermint to make lsh might be yielding less then expected. The chlorine in tap water, I know SWIM used tap water when he did the extraction, is destroying the product. Oh well too late. SWIM is growing HBWR as well but it's only in it's first year and won't yield any seeds this time around. Good luck yourself, thanks again.

damiana

 

[Observant]

After much experimentation with many failures and few successes a few things have been realized / concluded.

1) Aqueous ammonia seems to result in an inactive product. (It may be just overshooting the pH? or something else?)

2) Sodium Bicarbonate works wonderfully for precipitating active alkaloids, however getting a product without residual baking soda is tricky.

So after a few hundred A/B and B/A attempts, a new direction was decided to be attempted.... Freeze precipitation.

While it is a crude method... The results are consistent, and the process is simple, and yields a rather clean product.

So... The process:
1) Powder seeds.
2) Soak in 80+% grain alcohol (only tested with food grade), with dash of acid.
3) Decant / Filter to achieve a transparent yellow liquid.
- Optionally evaporate down to 10% of volume (will improve precipitate size
and efficiency of the pull.)
4) Drop it in a VERY cold freezer for 5-10 days. (White precipitate will form!)
5) Filter (in the freezer), or in the presence of dry ice.
- If it gets warm during the filtering, the precipitates will re-dissolve.
6) Enjoy the lsx crystals, or put into solution.


This could be done with many other solvents. For a more pure product, a few initial defats would help.

Without the defats however, the precipitate is white/clear and pretty damn potent.

Well can't be precise as the most accurate measuring tool readily available is .01 g. With the evaporation down to ~10% of initial pulled volume about .06% of initial dry morning glory seed.

So I'd say that's about 60% efficient based on the asumption of .1% by weight actives.

The obvious benefit of such a method is to never be working with the freebase form, which is much less stable.

Through some experimentation it has been found that the precipitated salt is still quite delicate. If not working with innate atm / vacuum etc, it is unwise to dry out the precipitate/filter. Generally the filter will take ages to dry if the ethanol is kept cold enough (evaporation nearly stops). The wet filter (or cotton ball as discussed earlier by JP) can have the actives extracted off with the use of minimal ascorbic buffered solute.

This solution is generally oxygen tolerant - however light is still a huge factor, the solution will come out clear-light yellow tint and glow vividly under black light initially. After 1 hour sun exposure said solution will turn dark green, unresponsive to blacklight, and inactive in bio-assay.

While the yields are short of amazing, the simplicity and reliability come in for the win. Even if an inert atm environment and a quality vacuum apparatus are readily available, working with such is rather tedious.

 

[burnt]

In theory one could make crude morning glory extract run it over a silica gel column (fine particles) get LSA. I'd recommend finding articles on the chromatography of these mixtures. The main problem is stability.

 

[panoramix]

Do you think something like this could work ?


1. Make paste from Powdered Seeds and Sodium Bicarbonate
2.Let it dry completely
3.Extract with non polar Solvent (Xylene / Acetone)
4.Add Fumaric or Tartaric Acid Saturated Acetone to make the Alkaloids drop out
5.Pour through coffeefilter.


or this one


1. Make a paste by mixing the Powdered Seeds with Sodium Bicarbonate.
2.Let the Paste dry completely
3.Extract with anhydrous Isopropyl Alcohol
4.Let the Isopropyl Alcohol Evaporate completely in Evaporation Dish
5.Redissolve in measured Acidic high proof Ethanol (possibly with Peppermint Extract)




What do you think ? The Freebase LSA might degrade too fast :/

some one allreddy tridfe this if not i wil do it tomorrow to test it oud have about 1kg of hbwr seeds so ill try