• If you have a question about commercial production or the hot sauce business, please post in Startup Help.

making extract with a soxhlet apparatus

ive seen several people talking about making pepper extract, so i thought id share how i go about it.

here's the soxhlet apparatus. it consists of a soxhlet, the bit in the middle. a condenser, the bit on the top. and the flask, the bit on the bottom.
here is what happens, once the flask is heated vapors travel up through the soxhlets sidearm up into the condenser, which condenses the vapors back into a liquid wherein they fall back into the soxhlet. the soxhlet is designed such that it will fill up with solvent and then drain itself almost completely back into the flask. it accomplishes this by starting a siphon once it begins to overflow through the small u shaped siphon tube you see on the side, this siphon will not break until it sucks air so naturally it empties almost completely. this process will cycle pretty much indefinitely as long as you provide heat and cool water to the condensor.

IMG_2128.jpg


heres the pepper we are extracting, dried bih jolokia pods, i have hundreds of them, id probably have more if the plant didnt catch a virus :eek: or atleast what i think was a virus.

IMG_2122.jpg


anyway, i tossed a bunch of these into a blender untill they were reduced to flakes

IMG_2123.jpg


these flakes were packed into a glass thimble, which is basically a container with frited glass disk on the bottom that allows solvent to drain through. you absolutly do not need a thimble, alot of people just stuff a bit of loose cotton or glass wool into the base of the siphon tube. keep in mind tho that w/e you are extracting will float, so you need to get a plug of cotton on top of w/e you are extracting so that it will not float around

IMG_2126.jpg

IMG_2132.jpg


and now we fill the flask... with 200ml of n hexane, good and cheep non polar solvent. we use hexane because its non polar, a non polar substance is not misicible into water hence it will not extract water soluble stuff like chlorophyll and w/e else is is in plant tissue. im not the person to teach you why things are polar and why things are not, but i can tell you that it has to do with molecules dipole moment.


IMG_2130.jpg


and now we apply heat! hexane boils quickly, at 70c. notice those little black bits on the bottom? those are boiling chips, i use them to get nice even safe boils. theres a phenomenon called "bumping" wherein you heat a liquid past its boiling point and it explosivly boils over at some trigger... like a bump. if you are lucky you just get a boil over into your distillate, if you are unlucky you get burned. you see 'bump flasks' on some apparatuses to stop contain this.

IMG_2137.jpg


soxhlet filling up...

IMG_2148.jpg


almost full...

IMG_2152.jpg


IMG_2153.jpg


to many photos!
 
ah, thats cool. keep in mind a gram isnt much. what i had in that photo was about a gram.

anyway heres an excerpt from a paper i have... if i could share it i would. but idk how to share pdf's?

Manufacture of oleoresin Capsicumor paprika –a global overview
As early as in 1949, Goldman described methods for the preparation of spice oleoresins, extracts
of red pepper and paprika, by extraction with Me2
CO or EtOH, filtration and removal of the
solvent by distillation. Soaking the cake before extraction improved the yield. A diagram of a
commercial-size extraction apparatus based on a Soxhlet method is given in his report. Berry
(1935) reported the examination of the extractives of Capsicums. The oleoresins of Capsicumvary
in appearance, solubility and degree of pungency according to the solvent used for extraction.
Et2
O and alcohol extract much of the non-pungent matter from chillies.
Ferns (1961a,b) compared various methods of extraction of oleoresin from Capsicum. A
laboratory-scale counter-current apparatus was found to be the best method. Acetone was
selected as the best solvent for the extraction of oleoresins from Capsicum.
Tandon et al. (1964) from CFTRI discussed the preparation of oleoresin of Capsicum(red
chillies) as well as its technological and chemical properties.
Szabo (1969, 1970) discussed the manufacture of paprika oleoresin and Mathew et al. (1971a)
covered in detail the preparation and quality control of oleoresin Capsicum. There are other
reports on oleoresin from Hungarian paprika and there is a Japanese patent on cayenne pepper
extract.
Blazovich and Spanyar (1969) described a method for the determination of capsaicin in oleo-resin and some other preparations with a high capsaicin content, while the gas chromatographic
detection of the acetone content of paprika oleoresin has also been reported. Govindarajan and
Ananthakrishna (1970) described the separation of capsaicin from Capsicumand its oleoresin,
Copyright © 2003 Taylor & Francis
and Mathew et al. (1971b) developed an improved TLC method for the estimation of capsaicin
in Capsicumoleoresin.
 
i got a beautiful clear orange liquid after using the 99% isopropyl alcohol, and added salt just to make sure there wasn't any water in it :D yay it didn't separate! i poured it off and it's drying now
 
it's slightly toxic but boils off really low and evaporates at room temp, and cost me about 50 cents to make that. i boiled it off by leaving the pyrex dish on top of my grill while smoking peppers.

yeah i didn't filter it, i don't really mind the organic particulate. time isn't a factor for me. i don't have that kind of money to invest in something i'd only use a handful of times... if i wanted to invest i'd go the cryogenic route.
 
those are nice little fractionation and simple distillation setups. those would work for recovering solvent, but unless you wanted to also distill stuff that required sharp fractions, id just get the second one. you can always get another column later if you need it.

i dont know how to make videos tbh. my phone has a camera, and so does my point and shoot, but idk how to edit and do voice over and stuff like that.

there is actually a number of videos of soxhlet operations on youtube already.

heres one.
keep in mind you dont NEED a heating mantle... but they are the easiest to use. one could always just use mineral oil or even vegetable oil baths. make damn sure you know what the boiling point of the oil is, you do not want your bath to boil!
 
Back
Top