Anyone want to test a homemade extract prep?

[StinkWeed]

Hey guys!
It might be a long time before I'm in any position to do this, but is anyone on here capable of doing an analysis (not by consuming it haha, I was thinking chromatography or something similar) on a homemade extract I occasionally have made for something like 10 years now? I don't have access to the equipment to make it via CO2 extraction, and so use N- Hexane, in small batches, purging it in a similar fashion to another product I have made with another therapeutic plant for close to the same amount of time. I made a thread years and years ago about it, and creating a more bioavailable p
final product with it before the forums relocated to this url, and was met with a pretty mixed response on the safety of the finished product (in others' opinions). I am really curious to see exactly how safe it is, and if it is comparable in composition to other extracts found to be totally safe. If anyone is capable of testing it for me please let me know! It might take a long time to ever go through with it but it is something I am very interested in finding out.

 

[The Kap'n]

This is extremely interesting. With all the equipment becoming more and more available these days I’ve been waiting for someone to get into a homelab hydrocarbon extraction. Much respect to you guys who have the talent to produce extracts in such a way.

 

[verticity]

Using n-hexane to extract kavalactones does not seem like a good idea. KLs are less polar than things like THC, so they can be extracted much more efficiently with ethanol. They are actually not very soluble in hexane. Flavokavains are less polar, so a kava extract made with hexane would likely have enhanced FK content relative to KLs. Ethanol also has the advantage of being food safe, which hexane is not. Hexane is made from petroleum distillate, so unless it is extremely pure, it's likely to contain trace amounts things like benzene, toluene, etc.. The only way to detect trace level contaminants like that would be by a fully equipped lab using GC or something..

Really the only food-safe method for making extract that I would recommend would be either water-only (this can be done with increased temperature/pressure) or ethanol/water (at least 50% water in ethanol will cause the FKs to precipitate out...). I suppose you could try d-limonene, which would be food safe, but that would also likely not be polar enough and extract too many FKs. (IMO d-limonene would be a good alternative for extracting active ingredients from "other therapeutic plants"...)

 

[verticity]

As an illustration of what I mean, here is a TLC slide showing the KL/FK content of extracts made using various solvents. To make this they made extracts with each solvent, placed a spot of each extract at the bottom of the slide and then dipped the bottom edge in a mobile phase. As the mobile phase moves up the slide, the extract separates out into it's components. The FKs go to the top, because they are more soluble in the non-polar mobile phase (which is methylene chloride in this case), and the KLs are spread out below. Tracks 6 and 13 are hexane extract, and you can see that the FKs are well extracted, but the KLs are much fainter than in the extracts from other solvents..for example ethanol (Tracks 5 and 12)
(Reference: Lhuissier, Tiphaine, et al. "Colorimetric assessment of kava (Piper methysticum Forst.) quality." Journal of Food Composition and Analysis 59 (2017): 27-34.)

 

[recentreturn]

As an illustration of what I mean, here is a TLC slide showing the KL/FK content of extracts made using various solvents. To make this they made extracts with each solvent, placed a spot of each extract at the bottom of the slide and then dipped the bottom edge in a mobile phase. As the mobile phase moves up the slide, the extract separates out into it's components. The FKs go to the top, because they are more soluble in the non-polar mobile phase (which is methylene chloride in this case), and the KLs are spread out below. Tracks 6 and 13 are hexane extract, and you can see that the FKs are well extracted, but the KLs are much fainter than in the extracts from other solvents..for example ethanol (Tracks 5 and 12)
(Reference: Lhuissier, Tiphaine, et al. "Colorimetric assessment of kava (Piper methysticum Forst.) quality." Journal of Food Composition and Analysis 59 (2017): 27-34.)
View attachment 8841

I don't understand all of this; so I will just ask the following question: Is it more dangerous to extract FK with the KL in an extract than to eat micronized kava (particularly if you were making your extract from a micro)?
*Edit: I am curious about the answer to this question but am also hoping that asking it won't hijack the intention of the original poster in asking the question and turn it into a different topic.

 

[kastom_lif]

Could butane maybe be a safer solvent? It's another popular one used for, uhh, therapeutic plants

 

[verticity]

Could butane maybe be a safer solvent? It's another popular one used for, uhh, therapeutic plants

Butane is explosive, so it is not safe for the person doing the extraction. But if you don't blow yourself up, the resulting extract would be less likely to contain toxic impurities. However, for kava it would have the same problem as hexane: butane is nonpolar and would not extract KLs efficiently.

 

[verticity]

I don't understand all of this; so I will just ask the following question: Is it more dangerous to extract FK with the KL in an extract than to eat micronized kava (particularly if you were making your extract from a micro)?
*Edit: I am curious about the answer to this question but am also hoping that asking it won't hijack the intention of the original poster in asking the question and turn it into a different topic.

For noble kava, FKs are not present is sufficient amounts to be harmful if you are consuming the whole root. So consuming micronized kava, which does contain small amounts of FKs, is not harmful. I would also not expect an alcohol extract of noble kava to have harmful FK levels. The problem with hexane is that I am afraid it would tend to concentrate the FKs and extract less of the KLs. That would mean you would have to consume more FKs to get the same dosage of KLs relative to micronized. Would those FK levels actually be harmful? I'm not sure, but FKB has been shown to be toxic in vitro, so I think it is best to play it safe and avoid extracts with high FK levels.

 

[kastom_lif]

Butane is explosive, so it is not safe for the person doing the extraction. But if you don't blow yourself up, the resulting extract would be less likely to contain toxic impurities. However, for kava it would have the same problem as hexane: butane is nonpolar and would not extract KLs efficiently.

 

[StinkWeed]

Using n-hexane to extract kavalactones does not seem like a good idea. KLs are less polar than things like THC, so they can be extracted much more efficiently with ethanol. They are actually not very soluble in hexane. Flavokavains are less polar, so a kava extract made with hexane would likely have enhanced FK content relative to KLs. Ethanol also has the advantage of being food safe, which hexane is not. Hexane is made from petroleum distillate, so unless it is extremely pure, it's likely to contain trace amounts things like benzene, toluene, etc.. The only way to detect trace level contaminants like that would be by a fully equipped lab using GC or something..

Really the only food-safe method for making extract that I would recommend would be either water-only (this can be done with increased temperature/pressure) or ethanol/water (at least 50% water in ethanol will cause the FKs to precipitate out...). I suppose you could try d-limonene, which would be food safe, but that would also likely not be polar enough and extract too many FKs. (IMO d-limonene would be a good alternative for extracting active ingredients from "other therapeutic plants"...)

Hey thanks for the input! I believe that was a response that came up the last time this was brought up, and a partial reason I'd like it tested (and why I said not by consumption haha). I agree with the idea of an ethanol extract being plenty safe using a noble product like a good micronized, and can at LEAST confirm that you get a significantly higher yield using ethanol and a vacuum funnel (or an aeropress type device) but I really don't often make any extraction anymore because it's plenty convenient enough just to get some micro or just BUY a nice extract that tastes much nicer if you really need it. You also don't have to go through a slow and more complicated purging process because what the heck are the minute amounts leftover going to do to you? It's 100 proof vodka lol. What you get with the hexane yends to be significantly lighter in color, and even using as pure of hexane as you can find online or your local chem store (NOT hardware store stuff), mixing the original evaporated substance gained into ethanol to evaporate once more, and then vac purged on a warming plate at a lower temperature, has a very strong, and different smell than the ethanol extract. It seems to pull different things than butane does, too (which is something I used to use for extractions with a cooled vessel to soak the material being extracted from in... Before my friends set themselves and their apartment on fire years ago, and I decided unless you actually have a totally closed off extraction set-up like a tamisium extractor or something it definitely isn't worth messing around with). So I'd like to know what's in it. I am now interested in an analysis of an ethanol extraction too, one with the usual 100 proof, and now you have me interested in what something like strong everclear will pull in comparison.

Edit: I did have another question, because I'm not a chemist. Is CO2 not ALSO nonpolar? I think I remember this being brought up as well last time.

 

[StinkWeed]

As an illustration of what I mean, here is a TLC slide showing the KL/FK content of extracts made using various solvents. To make this they made extracts with each solvent, placed a spot of each extract at the bottom of the slide and then dipped the bottom edge in a mobile phase. As the mobile phase moves up the slide, the extract separates out into it's components. The FKs go to the top, because they are more soluble in the non-polar mobile phase (which is methylene chloride in this case), and the KLs are spread out below. Tracks 6 and 13 are hexane extract, and you can see that the FKs are well extracted, but the KLs are much fainter than in the extracts from other solvents..for example ethanol (Tracks 5 and 12)
(Reference: Lhuissier, Tiphaine, et al. "Colorimetric assessment of kava (Piper methysticum Forst.) quality." Journal of Food Composition and Analysis 59 (2017): 27-34.)
View attachment 8841

This is super cool. I was thinking something more like GC, though. I get what this shows, however I'd kind of like someone who has tested some of the more popular available extracts to run a similar test on the hexane extract, the 100 proof (which you and I seem to think is probably the best bet, funny how different this plant is than C. Sativa lol, that plant gets a quick, freezing extraction on cold material while this gets a longer exposure at a warmer temp because the final product is not being combusted, and therefore chlorophyll and waxes are not nearly as "undesirable".) and an extraction with a very high proof ethanol solvent (like everclear). That way they can weigh in on content and whether or not it comes out as safe for regular consumption. I would just send it in to a lab nearby that does tests on other extracts, but I'm pretty broke .

 

[NileKinnick]

Using n-hexane to extract kavalactones does not seem like a good idea. KLs are less polar than things like THC, so they can be extracted much more efficiently with ethanol. They are actually not very soluble in hexane. Flavokavains are less polar, so a kava extract made with hexane would likely have enhanced FK content relative to KLs. Ethanol also has the advantage of being food safe, which hexane is not. Hexane is made from petroleum distillate, so unless it is extremely pure, it's likely to contain trace amounts things like benzene, toluene, etc.. The only way to detect trace level contaminants like that would be by a fully equipped lab using GC or something..

Really the only food-safe method for making extract that I would recommend would be either water-only (this can be done with increased temperature/pressure) or ethanol/water (at least 50% water in ethanol will cause the FKs to precipitate out...). I suppose you could try d-limonene, which would be food safe, but that would also likely not be polar enough and extract too many FKs. (IMO d-limonene would be a good alternative for extracting active ingredients from "other therapeutic plants"...)

What would you use for ethanol that's readily available? Any liquor is going to be, unless I'm mistaken (I'm no scientist), minimum 40 proof/20% ABV if you mix 1:1 with water. Or is the idea that you let most of the liquid evaporate so you're left with a very concentrated liquid with less alcohol (or do kavalactones evaporate with water and alcohol)? Please forgive me if all of this sounds dumb. I studied math in college and 0 chemistry/physics after high school.

 

[verticity]

...What you get with the hexane yends to be significantly lighter in color, and even using as pure of hexane as you can find online or your local chem store (NOT hardware store stuff), mixing the original evaporated substance gained into ethanol to evaporate once more, and then vac purged on a warming plate at a lower temperature, has a very strong, and different smell than the ethanol extract....

The lighter color is probably just because it extracts less of the kavalactones, some of which (Y and DMY) have a visible color.

... Before my friends set themselves and their apartment on fire years ago...

Oy. I hope your friends are OK... Butane is bad, m'kay?

Edit: I did have another question, because I'm not a chemist. Is CO2 not ALSO nonpolar? I think I remember this being brought up as well last time.

The quick answer is, yes CO2 in the gas phase is mostly non polar, but in the supercritical state, strange things can happen and it can act as a semipolar solvent. The longer answer: Basically, normally CO2 is linear like O=C=O, a carbon in the middle, with an oxygen on either side. Oxygen is more electronegative than carbon, so something like carbon monoxide, C=O is polar because the oxygen end is more negative than the carbon (the oxygen tends to attract electrons toward itself). But CO2 is symmetric so is non polar. But what I think can maybe happen at high temperature/pressure in the supercritical state is the CO2 can vibrate a lot, so it spends more time in a "bent state": picture the O=C=O flopping around so the oxygens and carbons are not on the same line, and also stretching in an asymmetric way so one oxygen is farther away than the other, like O===C=O. Those are called excited vibrational states, and in those states CO2 is somewhat polar, so if it spends enough time in those states, it would become better at extracting things that are not strictly nonpolar. You can tune the temperature and pressure of a CO2 apparatus to optimize extraction of various things such as KLs, so in theory you could tune it to maximize KLs and minimize FKs. I have not seen any test results of FK/KL for CO2 extracts so I'm actually not sure how that works out in practice.
(Reference: https://ocolabs.com/technical-supercritical-co2-details/ )

What would you use for ethanol that's readily available? Any liquor is going to be, unless I'm mistaken (I'm no scientist), minimum 40 proof/20% ABV if you mix 1:1 with water. Or is the idea that you let most of the liquid evaporate so you're left with a very concentrated liquid with less alcohol (or do kavalactones evaporate with water and alcohol)? Please forgive me if all of this sounds dumb. I studied math in college and 0 chemistry/physics after high school.

IMO, a mixture of ethanol and water is better to use for two reasons: the water will extract water soluble chemicals like glutiathone, which are probably beneficial, and also the water mixed with the ethanol will minimize FK extraction.

But if you actually do want high proof ethanol, Everclear is 190 proof (95%)... to get 200 proof you would have to use fractional distillation. Most of the industrial "ethanol" that is sold is "denatured" with stuff like methanol and isopropyl alcohol, so that stuff is not safe to use for extracts...

 

[Zaphod]

Hmmm, I have some 190 proof Everclear left over from the holidays (I like making my own Kahlua with it...). Are there any good references out there for making an ethanol extract? Previous threads maybe? I could easily mix up some kava with a 50/50 mix in a mason jar and let it sit for a while. The questions I would have:
(1) What is a good ratio of solvent to kava?
(2) how long would extraction take?
(3) Would heating speed up the process?
(4) Once extracted would you want to evaporate off some of the 50/50 mixture or use it as-is?

 

[StinkWeed]

Q

The lighter color is probably just because it extracts less of the kavalactones, some of which (Y and DMY) have a visible color.

Oy. I hope your friends are OK... Butane is bad, m'kay?


The quick answer is, yes CO2 in the gas phase is mostly non polar, but in the supercritical state, strange things can happen and it can act as a semipolar solvent. The longer answer: Basically, normally CO2 is linear like O=C=O, a carbon in the middle, with an oxygen on either side. Oxygen is more electronegative than carbon, so something like carbon monoxide, C=O is polar because the oxygen end is more negative than the carbon (the oxygen tends to attract electrons toward itself). But CO2 is symmetric so is non polar. But what I think can maybe happen at high temperature/pressure in the supercritical state is the CO2 can vibrate a lot, so it spends more time in a "bent state": picture the O=C=O flopping around so the oxygens and carbons are not on the same line, and also stretching in an asymmetric way so one oxygen is farther away than the other, like O===C=O. Those are called excited vibrational states, and in those states CO2 is somewhat polar, so if it spends enough time in those states, it would become better at extracting things that are not strictly nonpolar. You can tune the temperature and pressure of a CO2 apparatus to optimize extraction of various things such as KLs, so in theory you could tune it to maximize KLs and minimize FKs. I have not seen any test results of FK/KL for CO2 extracts so I'm actually not sure how that works out in practice.
(Reference: https://ocolabs.com/technical-supercritical-co2-details/ )

IMO, a mixture of ethanol and water is better to use for two reasons: the water will extract water soluble chemicals like glutiathone, which are probably beneficial, and also the water mixed with the ethanol will minimize FK extraction.

But if you actually do want high proof ethanol, Everclear is 190 proof (95%)... to get 200 proof you would have to use fractional distillation. Most of the industrial "ethanol" that is sold is "denatured" with stuff like methanol and isopropyl alcohol, so that stuff is not safe to use for extracts...

Thank you! I've always wondered why I see co2 extracts of kava and how they are feasible in an economical sense... My female friend essentially woke up in icu. I visited them there and they described the explosion and aftermath and I saw under the dressings... As an added deterrent to anyone here who might be thinking of using butane (or still do) for their other herbal extractions... My male friend said once the explosion happened his girlfriend's synthetic fiber jacket essentially fused to her skin while still flaming, leaving her horribly burned, he was not wearing a jacked, and yet said it looked like he had been... The skin from his arms literally fell off of his arms while still burning. Butane is EXTREMELY dangerous to work with that way, burns extremely hot, and they were outside, too. I can only imagine what it's like for people who are foolish enough to try that indoors