Extraction of 95+ % purity Salvinorin A from Salvia divinorum leaves
There are many TEKs around since ~ 20 years to extract Salvinorin A from Salvia leaves. Even though I tried some of them I never had too much luck ... the result was never truly crystalline and therefore not pure. In every case the separation from Chlorophyll was the nemesis. The IPA re-x should serve this purpose and it is confirmed to do this job, but for me it never truly worked. If you want to give this other method by Loveall a go, check
here. It is also confirmed that it can give a white crystaline product! Now here is a different TEK which will deal as efficient as possible with the removal of Chlorophyll. It requires a little more chemistry equipment than the regular extraction TEKs, but it is designed to still be 100 % kitchen friendly. If you want your hands on pure Salvinorin A, then just grab these goodies!
Comment:
The title says 95+ % Salvinorin. I am pretty sure it is basically pure Salvinorin, but currently I can only measure NMR myself and this is not 100 % accurate to be used as a purity value as Integral-% is not necessarily purity-%. I am waiting for a GC/HPLC measurement from a friend and then the title will be updated. 95 % is more of a conservative guess to not overshoot
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Table of contents:1. TEK
2. TEK in Short + Solubility Table + Q&A 3. Analytical Data (NMR so far only, more coming)4. Crystal microscopy5. Chemical Properties of Salvinorin A (like Evaporation Temp for your Crystals) can be found
here.
What do you need?- 100 g dried Salvia Leaves
- 2 L dry Aceton
- 3 g activated Charcoal (I used 0,3-0,5 mm, 35-50 mesh ASTM)
- 50 ml Methanol (not IPA)
- 1 L container with seal
- Smoothie mixer (or hands + knife
)
- small 1-way plastic Flash Column or any cylindric glass with ~ 2 cm diameter
- Hand Centrifuge like
this. Dont worry it's cheap and still even optional only, but will increase yield.
- Pestle and Mortar
You can get the column in any chemistry store.
This is an online example. Dont worry. Price is for 50x pieces because they only sell bulk. You will only need to buy 1x very cheap at a local chemistry store ... or find any other vessel that is a ~ 2 cm cylinder, which can hold a package of grains.
TEK:
1. Extraction from the dried LeavesPut your 100 g leaves into a smoothie mixer in packages of 10 g each. Turn on smoothie mixer on lowest setting for only 1 second. Leaves will be shredd into ~ 1 - 5 mm size. You dont want them to be too small, as this will make decanting of extraction solvent too laborious. Smaller leaves will need less solvent while making the whole process more efficient. If you dont have a smoothie mixer, use any other grinding machine that you can get that does NOT produce fine powder. If you have nothing by hand ... just use your hand
. Fill your leaf material into the 1 L bottle. If leaves are cut small enough, they might only fill 50 % of the bottle. Now fill the plant material with Room Temperature Aceton (
YES you read right - for this TEK it does not need to be Freezer-Temp. Check Q&A) until the plant material is completely covered. It will be ~ 400 ml. Now shake the vessel for 60 seconds. Decant any liquid while using a sieve to not let any plant material leave your glass container. Now repeat 3 times with fresh Aceton to do a total of 4x Room Temperature Extractions.
Picture of the shredded leaves. The 10-Cent Coin is for Scale with 20 mm diameter (left) Aceton bottle after extracting from the leaves. Colour is dark green.
Now you will need to let all the small particles settle that we also took over into the Aceton. The leaves are full of dust or small particles and structures located on the leaves like Trichomes. Filtering is barely possible, so just let it stand for 5+ hours and then decant. You may filter the residual liquid as this now will be much faster.
2. Washing your crude Extract with Naphtha-- According to Famine this whole step might be unnecessary ... You might directly move on to 3. and then report here if you still got needle-shaped crystals at the end --
This part is the same like in other TEKs. Evaporate your Aceton Extracts. When using a fan, evaporation will be really fast and therefore cool down the liquid due to the heat uptake of the transition liquid -> gas. Therefore water will condense into the liquid and take longer at the end to evaporate as a downside.
Resulting dark-green powder: ~ 1,1 g (1,1 %).
This consists of Salvinorin A + Chlorophyll + plant
fats. In the isolation of nature products the term
fat does not necessarily speak of real Carbohydrates, but of any components that are disregarded by our extraction desire, but will be carried along the extraction pathway and we need to get rid of them. Still, most of them are non-alkaloids and only soluble in organic solvents like
real fats (or Salvinorin
). This step will remove a lot of these unwanted compounds and a little Chlorophyll.
With Hand-Centrifuge:
Put your dark-green powder in a centrifuge tube of correct size and fill the tube up with Naphtha. Regular sizes would be 15 ml which is perfectly suited. Fill another tube with 15 ml Naphtha as the
anti-weight. Now shake your Plant-Extract in Naphtha inside the Tube to evenly mix and let the Naphtha soak up as much
fats as possible. Then put the tube and anti-tube inside of the hand centrifuge and start rotating. You will not need too much power to get all the plant material down. The first time it will be hard to see the bottom centrifugate but just decant it and it will have worked. If there is no centrifugate fill the liquid back inside and go faster/longer this time. Repeat until the surfacting liquid has a pale colour. Dont worry: it will never become clear. Just compare to the following picture.
No Hand-Centrifuge:
Dont worry, check the Q&A.
Picture of the extracted Plant Material, containing Salvinorin A, Chlorophyll and Fats (left). Centrifuge tube before (top) and after (bottom) a rotation round (right). The bottom picture shows the colour which you get at maximum with this method. A more clear Naphtha is impossible so dont worry it will be fine.
Now let the Naphtha evaporate.
Resulting light-green powder: ~ 0,51 g (0,51 %)3. Complete Removal of ChlorophyllNow "complete" is a big word. It will remove 99,9 %+ of the Chlorophyl. Nature is a genious so it has designed this molecule to be the most efficient photo-trap you could imagine. That means it has an insanely high extrinction coefficient which means even a parts-per-million concentration will colour stuff green. Anyways this will not stop us from getting 100 % white crystals. To remove the Chlorophyl in a failproof way we will use a trick. And this is creating a cheap adsorption-column. Activated Charcoal is a perfectly adsorbing grain which is also used as a decolorant for pharmaceuticals. We will use it the same way and let our Salvinorin Solution run through a package of Activated Charcoal, fixed in a tube-structure. For this reason we either need this cheap 1-way plastic column or anything similar. Important is that you can fix the Activated Charcoal package inside of the tube and it will not just fall through. You might use cotton to make a stopper for creating your own solution. In this example I have Activated Charcoal with a size of 0,3-0,5 mm. This is still too big, as it creates a lot of air inclusions when pouring into the column. We would need to unnecessarily increase the Charcoal Amount. Instead grind it to a fine powder. Use 3 g of activated charcoal for 500 mg of Salvinorin/Chlorophyll extract. Dont worry, just go for 5 min of grinding. Dont worry: A pestle and mortar cannot produce infinitely small grains so you will most likely end up in the same volume range. Pour the Activated Charcoal into the Column. You want to create an even bed without valleys. Use 10 ml Aceton per 500 ml plant extract to dissolve your crude Salvinorin/Chlorophyll mix. Now pour this mixture through the activated charcoal. Collect what is coming out and wait until the drops are coming really slowly - you might not directly collect all 10 ml. Now pour in 20 ml of fresh Aceton and collect until drops are coming slowly. Repeat 2 times to wash your column with a total of 20 + 20 + 20 ml fresh Aceton. This will contain all your Salvinorin, while 99+ % of the Chlorophyl is stuck to the activated charcoal (Why is this working? Check Q&A). The colour of the Aceton will still be slightly green. But dont worry, as told above this is Chlorophyll in the ppm range of even less and you removed basically all. Compare with the following pictures.
Picture of the Salvinorin-Chlorophyll-Mix dissolved in Aceton. Take a look at the green to black colour (left). The same liquid after running through the activated charcoal package (right). The liquid is baiscally free of Chlorophyll. Take a look at the droplet just falling from the column. The black material you see at the top is the layer of 3 g finely ground activated charcoal.
Now let the Aceton evaporate. This is still not completely pure Salvinorin A, but you might stop here as you have a solid which can be perfectly handled.
Resulting light-green powder: ~ 0,45 g (0,45 %). 4. Recrystallization to Salvinorin A needlesNow we will use the Recrystallization, but not to get rid of Chlorophyll (still we will loose the last bit of green coloration here ...). This is performed in Methanol instead of IPA. Methanol is really dangerous to your body, so in case you dont like it you might use IPA as a last ressort. Place your crude Salvinorin inside of a beaker and crush it as fine as possible. Now cover it with 20 ml of Methanol per 500 mg of crude Salvinorin and boil it for 2 min - preferable while stirring. If nothing more dissolves, decant into another vessel. The Methanol will have catched up a slight green colour from the last traces of Chlorophyll. Repeat with 20 ml fresh Methanol. If there is still a white powder remaining that did not dissolve, you can crush it even finer and use a last 10 ml of boiling Methanol. If that does not dissolve it is not Salvinorin A. For exact solubility of Salvinorin A in Methanol see the solubility table at
this post. Solubility may vary depending on from what matrix you extract your actives.
Picture of the crude Salvinorin extract after removing the Chlorophyll. Only traces of it are left, causing a slight greenish colour (left). Picture of the Salvinorin, starting to precipitate as fine needles from the Methanol (right). Note how the Methanol now has catched up even the last molecules of Chlorophyll.
Now place your Methanol in the Freezer at -20 °C over night. Afterwards decant off the Methanol. The needles might be really delicate and small, so maybe a Filter will be needed. Wash the needles with some fresh Methanol which is -20 °C temperature.
You might evaporate the combined Methanol separately to get some more mg of Salvinorin A with a lower purity.
Resulting white needle-shaped crystals: ~ 0,291 g (0,29 %)Picture of the Salvinorin extract which we can call Salvinorin A now (left). Picture of the Salvinorin A crystals at the microscale (right).
Enjoy!
(I actually mean extracting, Salvia is hell of a drug so it cant be
enjoyed if you ask me
)