Kratom Acid-Base Extraction

OttoBulletproof

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Can naphtha be used for the extraction?
 

OttoBulletproof

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I tried following your steps today.
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30g of Kratom Leaf powder were added to a 1L Erlenmeyer Flask with 200ml of 5% Vinegar. The mixture was stirred on a magnetic stirrer for about 15 Minutes until there were no more clumps of Kratom powder.
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200ml of warm dH20 were added and the mixture was put into a hot water bath, temperature kept between 60-80°C.
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I didn't measure out the ammount of Sodium Hydroxide but I think it was around 7-8 Spoons. The mixture turnt red/magenta. I tried measuring the ph but the kratom always got on the ph stripes and made the results unclear so I just guessed.
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After an hour in the hot water bath I added 40ml of Naphtha.
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I poured the naphtha into the mixture, swirled around and let it sit for 15 Minutes. The naphtha got now really dark and was not see through anymore. I probably had an emulsion. I added some NaCl and tried breaking the emulsion with a vibrator app on my phone. I don't know if It fully broke tho. I put the naphtha into the dish and let it dry with opened windows and a fan.
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After two pulls I was only able to scape this ugly looking stuff out of the dish. Where did I go wrong?

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G.Patton

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Hi, sorry for a long reply.
Was these table spoons or teaspoons? I think it was too much.
Have you tried to use this stuff? Probably your product there in these oily snots. You just need to crystalize it. You can repeat procedure with xylene if you don't have toluene. Probably solvent play key role here.

Add table spoon of xylene to this product and try to scratch it by glass rod or fork on a ceramic or pyrex dish. Small crystals have to appear.
 

HIGGS BOSSON

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Kratom extract, which I bought for myself, looked exactly like this. They were not a crystalline powder, but looked like a thickened resin of almost black color.
 

OttoBulletproof

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Table spoons. I tried it like that and it had little but some activity. I've read that naphtha actually only extracts the fatts from kratom and only a negligible ammount of alkaloids. But it was fun trying out some amateur chemistry again. :)
 

JimmyyJammzz

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This is pretty neat. I'm a very junior chemist but this seems easy enough to not even be a challenge. I am excited to try it.
 

Agilent1100DAD

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@G.Patton I used to do quite a bit of kratom/kavalactone extractions. I was developing a 7-OH mitragynine sublingual drug delivery system for opioid dependence and a dihydrokavain transdermal patch for smoking cessation. The focus of this post will be on the kratom extraction, although the same “findings” on enhanced extraction methods can be applied to the kava. I wish I could remember enough of my procedure to write a full report… but nonetheless I’ll share some photos I took during the process. We also managed to come up with a good and robust quantitative analysis for the determination of alkaloids such as corynantheidine, 7-hydroxymitragynine, isocorynantheidine, mitragynine, paynantheine, speciociliatine, and speciogynine. We coupled a Agilent 1100 with a triple quad mass spec. The column was a Waters Acquity BEH C18 column (1.7 μm, 2.1 × 100 mm) and the mobile phases were ammonium acetate buffer (A) and ACN (B). We also developed a method for separation and quantitative analysis of most kavalactones such as desmethoxyyangonin, dihydrokavain, yangonin, kavain, dihydromethysticin, and methysticin; which was a real pain in the ass. I don’t have the chromatographs for the kava analysis unfortunately.

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I do remember managing to separate and collect about 50 mg of purified paynantheine via flash chromatography and it rocked my world. I wish the synthesis routes weren’t so complicated for these compounds!! Below is my make shift flash chroma system lol. I used a peristaltic pump with digital controls and a redisep flash column.

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Going back to the extraction of kratom, the best initial extraction method I found was to take the powdered kratom and add ethyl acetate to it. We used a 5L reaction flask a single 24/40 neck. We used a combination of sonication snd heat with a reflux condenser. The photo below has the kratom extraction set up to the left snd a kava extraction to the right.

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afterwards, we filtered, evaporated the solvent and did some sort of A/B extraction. We ended up with these dark green crystals, pictured below.

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Lastly, I remember winterizing/defatting the kratom and kava residue worked very nicely
 

G.Patton

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Can you tell me about chromatograms a bit more? I'm interested in the picture: are these chromatograms of each sample from one batch, are these different batches?
 

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G.Patton

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Hello, I need more input data to help you. Write here please your step-by-step procedure. Actually looks nice, recrystallize it.
 

Mr. F

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At first i tried to dissolve 40g of Kratom powder in 200mL of acetic acid 5%, which didn't work as expected because it was still Solid and Not in a soluted state, so i added another 200mL of the acid and stirred the mixture for a few minutes on a magnetic stirrer. Then i added 200mL of warm/hot destilled water and stirred for another Like 5-10 minutes.

Then i made the NaOH solution (but with normal water instead of destilled water because i didn't thougt of it, that the water in the NaOH solution should also be destilled 😃), and added like 300mL of it, because at first i used to less NaOH in the solution and the pH didn't increased so rapidly. The last pH mesurement was around 12-13, where the solution hat a dark Red to brownish colour.

After that i let the solution stirr for about an hour and keept it warm with the heating Plate on the magnetic stirring table.

I then added around 40mL of toluene stirred Well, and let the two phases seperate for a few minutes. I took of the toluene Phase with a Pasteurpipette (which was a hell of a procedere, next time i will use a seperating funnel ) and droped it into a flat Glas pyrex. I extracted two more times with 40mL of toluene.

I let the solvent evapruate over night outside, and then scraped the thin layer which was left with a razor Blade. I got a P
powder which was a bit darker than on the picture i posted.

I dissolved the Powder in Like 20mL of acetone, filtered it and again put it on the Glas pyrex. After Aceton dissolved i got this orange powder with a few crystals in it which smells floral as you decribed in the main post. I haven't weighed it yet because i want to do another Aceton wash, hopeing to get better crystals.
 
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Sir_Smokealot

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@G.Patton Can I also use xylene instead of toloul?
 

G.Patton

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Hello, what is it? Do you mean Toluen? Yes, I think xylene can be used.
 
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