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Pure cacsaicin from chilli peppers Answered

I already had a quite long Ible in the making when it downed on me that not too many people should actually create such a dangerous substance at home.
So instead I decided to just write a bit about the history, general procedures and what is possible or not.
If you already made your own chilli exptract for a special hot sauce or your home made pepper spray then you feel right at home.
Those who never done anything like it or at least some essential oil extractions might just find some other interesting stuff to read.
I won't go into all details here as those with the basic knowledge will already know the precautions and most things.

Capsaicin...
The stuff that makes your exes run, clear you nose and makes you sweat like you on fire.
At least if it comes within you favourite dish.
In the pure form it is a severe irritant and should be handled like explosives or concentrated acids.
You just won't make a mistake with this stuff twice - trust me!
What really harms you is not the capsaicin itself, it is your bodies reaction to it!
It stimulates the same nerves responsible to feel heat and pain, sometimes those for a severe itch as well.
And unlike a normal reaction you would get from hot water, it won't stop until it is fully removed.
Even after this the body keeps reacting for bit longer.
On the skin you can end up with blisters like from a real burn, in your airways it can make breathing impossible!
And lets just say that swimming goggles won't look as dumb and funny on your face once you realise you got some fine crystals on your face....
If you dare to continue then I assume you are well aware of the risks, dangers and PPE requirements!

Pure or extract?
I checked tons of so called instructions on how to make pure or 99% pure capsaicin from chilli peppers.
They all just produce a really crude mix of goo that happens to have a lot of capsaicin in it.
If it is red or even darker it is nowhere near pure.
If it has a weird smell that has really nothing in common with chilli than it is even worse.
If it is more or less colorless, with a very strong scent that your nose does not like at all then we are getting somewhere.
So why is it that we always end up with this color that is impossible to remove?

Extracting chilli peppers....
A thing most people ignore a bit when in a hurry is that an alcohol extraction requires DRY alcohol.
You just won't tolerate water in it, which is why often methanol comes easier and cheaper than ethanol.
Some people even think just because the alcohol is either evaporated or distilled off that all is good when using things like methylated spirit.
Ever had the problem that you used that stuff and your hot sauce made you vomit after realising that it comes with a bad and extremely bitter after taste?
That is the stuff that makes your home depot ethanol unuasable ;)
If you use homegrown or otherwise fresh chilli you need to fully dry it first!
Don't be fooled by people stating they did it with fresh peppers.
What you get this way is some of the worst extractions you can get.
Don't be fooled to think you need some Carolina Reaper either.
A big bag of chilli powder from your grocery store will do just fine.
So what is all in our extract?
Alcohol or any other solvent usable for a capsaicin extraction also dissolves a lot of other things.
Like the beta carotenes that give the extract the organge to red color.
The skin and the entire fruit also contains oils, plus the shiny outside is mostly due to wax...
All of this ends in your extract....
You not only get what you want and might not mind but also everything else you don't want.

Making the difference....
The impossible we do right away, for miricles or wonder allow a day or two of processing ;)
Assuming you end with a rather large qauntity of alcohol the concentration of everything is relatively low.
If you used something like a Soxhlet extraction you already degraded a lot of the capsaicin due to the heat.
And even after the best filtering you might have a clear solution but whatever is not a solid is still in there.
Imagine you would put it all into a freezer....
Surprisingly a lot of stuff won't stay in solution once cooled down enough.
Especially if you give it a few days.
Depending on what you started with you either get a slimy looking sludge or some crystals showing.
Either way it needs to be filtered out and washed.
For the washing use the same pure alcohol as before but make sure it is well cooled.
If any cacsaicin was already forming crystals then they will be washed into your solution again now to a little extend.
But you removed an awful lot of the wax if it was not capsaicin already. ;)

Testing the slurry we collected.
When using chilli powder from the shops I noticed that there is often no wax to be found at all.
While for fresh produce the content is significant.
Once dry you make a simple test with water.
Capsaicin basically does not dissolve in water, so it would sink to the bottom while wax floats ;)

I assume you ended with little to no wax but fine capsaicin instead.
From the natural form it is very hard to get crystals bigger than a dust particle.
This only happens if the temperature is cold enough and the concentration high enough.
As my entire setup is quite small I usually prepare several 500ml plastic bottles that I fill to one quarter by height with chilli powder and then fill up to half with methanol.
In the end I use a full 1kg bad of chilli powder but only a may of 5 to ten bottles.

Making the most of it.
When using alcohol extraction you want to use a little of the solvent as possible.
Use means here wasting it instead of recycling it.
Once I filtered my white slurry out I destill the remaining solution to reduce it by 50-75%.
An almost dark red color is usually when it is time to stop.
After this I place it back in the freezer for a day to check if more crystals or slurry forms.
If so then I filter it off again.
What is left is then mixed with recycled and fresh methanol to soak more chilli powder in my bottles.
Means I discard the filtered of chilli poweder once washed, recycle what I can from the methanol and keep whatever the slurry produces that is not wax or dissolves in water.
Depending with how much chilli you start you will get to the point where your filtered solution is already dark red.
Since the final capsaicin won't dissolve in water you can destill with some added (destilled) water.
This way you recover the alcohol without risking to get a sticky goo everyhwere that you need to clean off.
It is quite possible to get some more capsaicin this way as with the alcohol leaving it will participate out.
Simply filter the solution once the alcohol is recovered.

As the beta carotenes won't dissolve well in water either it is best to perfom this destillation while all is mixed.
If you can't do this then don't worry to much, it just means a few more minutes of cleaning later ;)

Testing the final product....
What you have left once the slurry is dried should be almost colorless with maybe a pale yellow in it.
Fully dried it should appear as basically white.
There should be no smell to it, nothing to tickkle you nose.
Colorless and odorless.
For whatever reason I still sometimes end up with a very faint smell.
Not really chilli though...
Depending on the temperature the products is either quite hard to almost britlle (when frozen) to almost wax like at room temp and above.
I highly recommend against testing whatever you have on your skin or to ingest it!!!
Waste some sauce base like ketchup (you can add it later to your sauce again) or some butter - I prefer the later.
Butter become liquid well below the 65°C celsius decomposition temp for capsaicin, so it should dissolve very easy in it.
Take a shot glass with just enough butter for a sandwich and dip a toothpick into your product.
Make sure there it a tiny bit on it and not that the toothpick has a thick coating!
Once cooled down while mixing every now then spread it on some sandwich and take a bite.
After a minute or two you should definitately feel a difference to just butter - hopefully not too hot.
If nothing happens repeat with a bit more on the toothpick.
Still nothing at all usually means you filtered out only by-products and for some reasons managed to make the capsaicin disappear.

Hints and tips that might safe your bacon....
Methanol boils at about 64°C, ethanol at about 77°C.
Capsaicin starts to decompose at 65°C.
Not a big deal but if you get to the 80° mark, which is easy which ethanol you might have to use evaporation instead of destillation and waste the alcohol to your surrounding air...
Water...
For the final product it is not a problem but during the extraction process it is.
Despite some people claiming otherwise both the quality and amount of what you end up with are lower.
It seems some of the capsaicin binds to the water molecules with the help of some other stuff that the plant material provides.
And when you try to destill a solution that was contaminated with water from the chilli it tends to foam up quite badly.
While with pure alcohol and fully dried product there is no foaming.
What to expect when collecting the end product...
At room temperature you can dissolve what you get in product from one kg of dried chilli powder in under 10ml of pure alcohol.
However at -20°C next to nothing dissolves in the alcohol.
That means as long as you have still over lets say 1000ml alcohol extract then very little will participate out.
Just one reason why I prefer to work with small batches - keeps the concentration higher from the start.
The more you destill off and re-use the higher the capsaicin concentration in the alcohol will be.
So before you start to add any water for the destillation you need to be aware of the consequences.
I found out that first destilling most of the alcohol off the single rounds that got too dark in color helps.
I just collect this conentrate for the final destillation process.
Key is to destill this off to the point where it just starts to thicken up a bit.
It should still be liquid but act almost like a thin oil.
You don't want it so thick that is crates a coating on the walls when you move the liquid around.
In case it did happen just add a tiny amount of alcohol again.
Put in the freezer for a few days....
Empty into your filter and let as much as possible drip out.
Rinse with as little alcohol as possible - have the rinsing alcohol at -20C as well .
Do not wash the filter with water but with the frozen cold rinsing alcohol.
Cover the filter up and leave in a cool place for the next run - have something under it as it might still let a drip or two off.
The remaining liquid leave to evaporate off until it just starts to thick up again a tiny bit - back in the freezer for a day or two.
Filter out again then while still a bit wet turn the filter over to remove most what is in it.
I prefer to empty onto a teflon sheet and to wear full PPE here....
While still wet you try to remove more from the filter with a fine but short brush, knife or whatever you find suitable.
Do not continue any action once the stuff starts to dry!
Place the filter into a sealed bag and leave in your freezer for when you do anthoer extraction - this way you loose far less product ;)
When doing a final destillation with added water to cover all the alcohol you are left with the remains of the original product, minus all solids.
Beta carotene is quite beneficial, so it would make sense to include it into your hot sauce.
Plus there will always be some leftover capsaicin in it.
If you want to use this part of the extract as well to really get what is possible then IMHO slow is better.
You can't just destill off or boil off the water to get a nice "sauce" base.
The capsaicin that is left would be mostly decomposed and with no effect anymore.
A clear sign of too much temperature is bad smell that really turns you off.
Hard to define in words but trust me, if you smell it you know what I means as you woul refuse to have this smell coming from your final hotsauce.
During the summer it no problem to just leave it out to evaporate in the shade !
You can do it in full sun but must make sure no sunlight gets into the liquid.
UV decomposes at least a lot of the karotenes....

Special equippment at hand?
If you happen to have a vacuum pump or at least a salvaged fridge compressor you can safe a lot of time.
A buchner filter for 500ml in the top is quite cheap but you can build something similar with a normal funnel.
Look it up it you want...
A proper buchner filter however already comes with a very fine glass filter built in.
Means you don't really need any filter paper - I still add it as it makes the cleaning easier.
Instead of waiting several hours for gravity to do its work on a coffe filter you are done in a few minutes.
Well worth trying out!
For the water destillation of the remaining end product, or by-product if you like, vacuum also helps.
CVD or Closed Vacuum Destillation sound complicated but is really simple.
One pressure vessel is filled with the solution to be conectrated, the other is kept empty.
Connected with a suitable pipe or hose and fully sealed.
The extract is heated to about 40°C while the empty vessel is placed into an ice bath.
With the pump and the help of a valve create just enough vacuum so create small bubbles in the heated vessel.
Close the valve and a few hours later there should be far less water in the hot one while the frozen one builds up ice.
Every now and then check the vacuum gauge and if require start the pump again.
You can do with just the pump and one vessel....
Problem is that the oil in your pump will quickly get far too contaminated with water.
You could add a conatainer with something like an absorbent but it would have to be sufficient for all the water you need to remove.
Most of all it must be able to absorb it fully before the airstream enters the compressor.
The benefit is that the capsaicin can't decompose at all.
In a vacuum or close to it anyways, a lot of the things that procude smell also disappear through the compressor.
Won't help it was already a stinky mess but will certainly reduce the smell of the concentrate.
If you prefer to keep this aroma for your final sauce then do not use a vacuum.

Why not a Soxhlet or similar device as used for essential oil extraction?
The benefit seems to be clear:
You have a relatively large vessel to hold a lot of chille powder and can let the alcohol cycle and wash it out completly...
Theory is not always reality.....
Firstly the alcohol runs through it many times while it dissolves what it can from the powder.
That means each round you actually wash with a higher concentration until there is equal amounts in the alcohol and the powder.
You waste about 50% of the end product unless you repeat it all several times with fresh alcohol.
Worst of all however is the temperature, even if you use methanol.
To make the alcohol evaporate enough to make the process work properly and in a timely fashion it must be heated to above 65°C, in most cases even with a proper heating mantle you won't have the temperature control tight enough.
It is quite possible to destroy 70% of the capsaicin this way....
The condesers used are also not really suitable for these low temperatures.
Means you should use ice water to cool.
Either way you will loose a lot of what could otherwise be product.

Funny things that might stumble you along the way.
In the freezer the solution will participate out a bit.
However, when back to room temperature most if it will still be there, only a fraction goes back into solution.
I could not figure out why this happens but once heated to about 40°C it all dissolves again.
Filter fully blocked by the product?
The fine sludge can be a problem even with a proper vacuum filtration unit.
Especially if the product is still not really a solid once fully dried.
A paper filter can be re-used many times but whatever makes it past and into the glass filter is tricky.
You should not get much here if the paper filter was fine enough but if it builds up to the point where it makes the filtration long and slow:
Remove the paper filter and add a small amount of luke warm alcohol.
If it does not start to trickle through already give it a minute or two before turning the vacuum on.
Starts a bit slow but should clear up quickly, if in doub repaet with a large volume of alcohol.
I prefer to do this cleaning before I start a new bag of powder or whever I need to restock.
Means I can use the same alcohol I had to clean the filter to add to the bottles with powder ;)
Nothing gets wasted if you are prepared....

If you find any typos in the above then feel free to keep them.
However if you decide to use the typos for monetary gain I would kindly ask for 5% of the net profit made from my typos.
;)

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