I recently ran into a thread talking about a soxhlet extraction kit, and it got me curious about all the goodies out there lab wise. I am not at all experienced in lab work but am very intrigued about it. What type of equipment would they use and such? Like how would they extract, recrystalize, seperate, etc... Any experienced science guys out there willing to entertain my question and curiosity?
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How would a professional lab extract DMT?
- Thread starter abrahamx
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blue.magic
Esteemed member
- Merits
- 42
The equipment heavily depends on what your tasks is (analysis, synthesis, microbiology etc.) and e.g. what quantities of what kind of substance(s) the lab should produce. Some labs are equipped only for analysis, not for producing anything. Microbiology lab has very different equipment from that used for organic synthesis.
In one you find Petri dishes, incubators, shakers and micro pipettes, while other will lack all this but have rotavaps, centrifuges and a vacuum line.
Extractions are done in Soxhlet and with exact amounts of various solvents to make an accurate measurements of the extracted substances and a repeatable process (required for later review by other chemists). You also don't want to lose or destroy any material in the process if you want to determine how much there is in a sample.
As for the psychedelic research, just look at some documentaries depicting Alexander Shulgin's lab. He had all the equipment for organic synthesis but his small lab was able to produce only small amounts of the target substance. Sometimes he worked months to obtain just 100 mg of some novel tryptamine.
Clandestine labs are a mix of dedicated tools (e.g. hotplate, distillation apparatus) and typical household items (pots, sieves etc.). These are targeted on cheap production.
LSD labs, on the other hand, demand lab grade equipment as one needs to handle dangerous and fragile substances. Careful measurements, safe handling and control over conditions are absulutely critical here.
In one you find Petri dishes, incubators, shakers and micro pipettes, while other will lack all this but have rotavaps, centrifuges and a vacuum line.
Extractions are done in Soxhlet and with exact amounts of various solvents to make an accurate measurements of the extracted substances and a repeatable process (required for later review by other chemists). You also don't want to lose or destroy any material in the process if you want to determine how much there is in a sample.
As for the psychedelic research, just look at some documentaries depicting Alexander Shulgin's lab. He had all the equipment for organic synthesis but his small lab was able to produce only small amounts of the target substance. Sometimes he worked months to obtain just 100 mg of some novel tryptamine.
Clandestine labs are a mix of dedicated tools (e.g. hotplate, distillation apparatus) and typical household items (pots, sieves etc.). These are targeted on cheap production.
LSD labs, on the other hand, demand lab grade equipment as one needs to handle dangerous and fragile substances. Careful measurements, safe handling and control over conditions are absulutely critical here.
I'm still a student but we are taught to seperate two phases with a separatory funnel. You could also pipet off the organic phase. The recrystalisation would probably take place in a flask on a hotplate stirrer with a reflux condenser. You would add a little of your solvent through your reflux condenser, just enough to moist the DMT, heat up to until the solution starts to boil, then slowly add solvent until the whole DMT is dissolved. Then you would cool it off to room temperature and finish the process with an ice bath. Now you would seperate the solvent from your crystaline DMT through a buchner funnel with the help of a vacuum pump and wash it with a little amount of solvent. Then of course dry it.
Additional steps like drying your solvent before using it or working under inert gas might be used but that's just a guess. Maybe re-x again depending on why the procedure would is done.
The above is based on what we're taught in the lab but it might not be the go-to procedure for seperating/re-xing DMT. I'm not even sure if there's an established method of extracting DMT. Usually it takes a lot of experience to figure out the best way to do things until they might even become a standard procedure. I have never extracted active compounds from plant matter so I'll just leave that unanswered. My bad.
Have you seen this thread? It might satisfy your curiosity: Learn useful chem techniques from MIT videos - FAQ - All your basic questions and answers - Welcome to the DMT-Nexus
Also I'm interested in answers of people that are more experienced in the lab or maybe even have performed a DMT extraction.
Additional steps like drying your solvent before using it or working under inert gas might be used but that's just a guess. Maybe re-x again depending on why the procedure would is done.
The above is based on what we're taught in the lab but it might not be the go-to procedure for seperating/re-xing DMT. I'm not even sure if there's an established method of extracting DMT. Usually it takes a lot of experience to figure out the best way to do things until they might even become a standard procedure. I have never extracted active compounds from plant matter so I'll just leave that unanswered. My bad.
Have you seen this thread? It might satisfy your curiosity: Learn useful chem techniques from MIT videos - FAQ - All your basic questions and answers - Welcome to the DMT-Nexus
Also I'm interested in answers of people that are more experienced in the lab or maybe even have performed a DMT extraction.
- Merits
- 117
Many ways to do it, and many ways have been used.. Two examples:
1
Matrix solid-phase dispersion (MSPD) (gaujac et al 2012)
An aliquot of herbal sample (0.5 g) was placed into a mortar
(ca. 50 mL), and 0.5 g of Florisil and 0.5 mL of NaOH 0.1 mol/L
were added. The sample was then gently blended into the sorbent
material with a pestle, until a homogeneous mixture was
obtained (ca. 3 min). The homogenized mixture was introduced into
a 100 mm ×20 mm id polypropylene column, filled with 0.1 g of
glass wool at the base and 0.5 g of anhydrous Na2SO4. The elution
was performed under vacuum with 30 mL of n-hexane. The eluent
was collected into a round bottom flask and concentrated using a
rotary vacuum evaporator (40 ◦C), and finally purged with a gentle
stream of nitrogen to a volume of 1 mL.
2
Standard A/B with defat (Gaujac et al 2013)
The powdered plant material (60 g) was suspended in 300 mL of 0.1 mol L− 1 hydrochloric acid in a glass beaker, and sonicated in an ultrasonic bath for 24 h at a constant temperature of 25 °C. The extract was separated by simple filtration and the residual material was washed twice with 300 mL using the same acid solution. The filtrates were combined, and the solution was washed with hexane to eliminate any plant oils that might be present. The aqueous solution was basified to pH 10–11 with 0.1 mol L− 1 NaOH, and then extracted with hexane (5 × 50 mL). The combined extracts were concentrated to dryness under reduced pressure to obtain the crude alkaloid. The solid resulting from filtration was air-dried, and recrystallized from hexane.
1
Matrix solid-phase dispersion (MSPD) (gaujac et al 2012)
An aliquot of herbal sample (0.5 g) was placed into a mortar
(ca. 50 mL), and 0.5 g of Florisil and 0.5 mL of NaOH 0.1 mol/L
were added. The sample was then gently blended into the sorbent
material with a pestle, until a homogeneous mixture was
obtained (ca. 3 min). The homogenized mixture was introduced into
a 100 mm ×20 mm id polypropylene column, filled with 0.1 g of
glass wool at the base and 0.5 g of anhydrous Na2SO4. The elution
was performed under vacuum with 30 mL of n-hexane. The eluent
was collected into a round bottom flask and concentrated using a
rotary vacuum evaporator (40 ◦C), and finally purged with a gentle
stream of nitrogen to a volume of 1 mL.
2
Standard A/B with defat (Gaujac et al 2013)
The powdered plant material (60 g) was suspended in 300 mL of 0.1 mol L− 1 hydrochloric acid in a glass beaker, and sonicated in an ultrasonic bath for 24 h at a constant temperature of 25 °C. The extract was separated by simple filtration and the residual material was washed twice with 300 mL using the same acid solution. The filtrates were combined, and the solution was washed with hexane to eliminate any plant oils that might be present. The aqueous solution was basified to pH 10–11 with 0.1 mol L− 1 NaOH, and then extracted with hexane (5 × 50 mL). The combined extracts were concentrated to dryness under reduced pressure to obtain the crude alkaloid. The solid resulting from filtration was air-dried, and recrystallized from hexane.
- Merits
- 42
What technique to be used largely depends on the quantity desired to extract. And also on the choice of the chemist/researcher.
If you have high end fancy equipment and just doing analysis, you might use a SPE matrix right into an HPLC, for microquantities.
Though, in general cases, the extraction performed and the efficiency of it is entirely dependent knowledge and choices made for a researcher, for example.
A standard method to isolate natural products might be to do a crude methanol extract, either by soxhlet or a simple soak and decant, followed by flash chromatography to isolate the compound. This method is very general and would work for a wide range of natural products, beyond amines like DMT. However, its difficult to scale up and is a tedious process and often results in a low yield of material that needs to be further purified. If there was no other information on the compound you wanted, you'd probably try this first.
The chemist/researcher probably understands DMT is an amine, but it isn't common to be able to easily extract even simple amine natural products from simple acid/base extraction, often it results in a gummy mess or terrible emulsion, which requires further purification and time spent. Or he may just try a simple acid-base extraction but waste time and effort with unnecessary defatting or extraction steps.
So the moral of the story is, do your research. If the chemist knows that DMT is cleanly extracted from an a/b extraction or from basic root bark soup in high yield and purity, then that is exactly what he will do. He might use a separatory funnel or a different solvent or use a sonicator to speed up the acidic extraction, but the rest remains the same as what is done here on the nexus.
There is a saying, 2 weeks in the lab is the same as one day in the library. Meaning, if you do your research you avoid walking into dead ends or reinventing the wheel.
The professional researcher would be delighted to find a source like the nexus, which is basically the hub of rootbark extraction research, there he would find answers and shortcuts he otherwise wouldn't have known, especially things the fumarate salts, otherwise would go through a lot of trouble to find what works well.
If you have high end fancy equipment and just doing analysis, you might use a SPE matrix right into an HPLC, for microquantities.
Though, in general cases, the extraction performed and the efficiency of it is entirely dependent knowledge and choices made for a researcher, for example.
A standard method to isolate natural products might be to do a crude methanol extract, either by soxhlet or a simple soak and decant, followed by flash chromatography to isolate the compound. This method is very general and would work for a wide range of natural products, beyond amines like DMT. However, its difficult to scale up and is a tedious process and often results in a low yield of material that needs to be further purified. If there was no other information on the compound you wanted, you'd probably try this first.
The chemist/researcher probably understands DMT is an amine, but it isn't common to be able to easily extract even simple amine natural products from simple acid/base extraction, often it results in a gummy mess or terrible emulsion, which requires further purification and time spent. Or he may just try a simple acid-base extraction but waste time and effort with unnecessary defatting or extraction steps.
So the moral of the story is, do your research. If the chemist knows that DMT is cleanly extracted from an a/b extraction or from basic root bark soup in high yield and purity, then that is exactly what he will do. He might use a separatory funnel or a different solvent or use a sonicator to speed up the acidic extraction, but the rest remains the same as what is done here on the nexus.
There is a saying, 2 weeks in the lab is the same as one day in the library. Meaning, if you do your research you avoid walking into dead ends or reinventing the wheel.
The professional researcher would be delighted to find a source like the nexus, which is basically the hub of rootbark extraction research, there he would find answers and shortcuts he otherwise wouldn't have known, especially things the fumarate salts, otherwise would go through a lot of trouble to find what works well.
Soxhlets are mostly aimed at hard to extrat compounds that need a lot of "pulls" or solvent.blue.magic said:
They arent aimed at accurate extractions really.
So you dont need to end up using tons of solvent and spending lots of time recycling it/ throwing it away.Wikipedia said:
Also its there to make long soaks obsolete so you just extract often with fresh solvent at elevated temp to make the extraction quicker they still take hours sometimes but its automated unlike lots of pulls and distilling.
Also its done hot (boiling point of solvent) which is not good for dmt so its not used for that.
Also it depends on mostly on scale and needed purity.
For example if you just want to check dmt yes/no a quick dirty 1 solvent crude extract is enough if you use accurate testing tools like thin layer chromatography.
For extracting large amounts of DMT a/b is the best way. A lab will probably use more expensive solvents tho and a quicker methology with higher security standards.
Then just purify. There are ofc better purifcation methods for labs like columns and vacuum distillation.
- Merits
- 42
Ulim said:
Couple things, chromatography is not a measurement tool, its a separation technique. What you can have is chromatography coupled with a method of detection, like mass spec.
Column chromatography is not 'better' as a purification method, typically they are worse than crystallization. And they require time and effort. They are only used to purify a crude product where other methods fail, like crystallization. Ideally, if you run a column, you want to recrystallize the purified material afterward. Crystallization is THE best way to purify anything, but often it is not possible in the given circumstances. Same goes for vacuum distillation, typically you might do that to purify an oil, something that cannot be crystallized at all.
Soxhlets aren't only used to extract a poorly soluble material, but also for quantitative extraction of plant material, for example, if you run a soxhlet overnight, instead of your regular 3 soaks, you do about 45 soaks with the soxhlet. Most of them are unnecessary but you don't mind because your sleeping, and you can be sure its a quantitative extraction of the plant material. So, definitely aimed at an accurate extraction.
Using a hot solvent for DMT is no problem because you're not extracting the freebase, you're using an alcohol to do a crude extraction on the salt forms of DMT in the plant material. Then you move to purify by other means, by acid/base, because its easier and more efficient to do an acid/base on a small amount of crude resin then it is to do on 10-100x the weight of plant material.
Mindlusion said:
i meant TLC and meant to use the word "Testing" afterall i did mean quantification and measuring just test for DMT yes/no
The rest was ment in "general"
And i do think chromatography is superior expecially if you have like 20 different compounds at different amounts.
