Sciencemadness Discussion Board - My piperine extraction setup without soxhlet extractor

My piperine extraction setup without soxhlet extractor

Syn the Sizer - 23-2-2020 at 10:41

Hello, this is my first post in this forum and thought I would show the setup I used to extract piperine yesterday. Now before everybody say "WTF are you doing man, chemistry in your kitchen", this is new glassware and has not been used for anything toxic short of a bit of HCl and NaOH. Also I an no stranger to extractions and evaporation using isopropyl alcohol indoors. With its decently high boiling point compared to my cold house I am confident no IPA fumes were escaping my rig but I did test periodically in for escaping gas as can be seen in my picture.

I realize I am probably not the first person to do this but I could not find a post about it. I did not have a soxhlet extractor but really wanted to extract piperine so I used my sep funnel in place of a receiving flask in a simple distillation setup and a round bottom underneath that. The sep funnel wasn't as hard to clean out as I expected and I was very satisfied with the results. It however did need periodic manual emptying of the receiving flask into the distillation flask. Its not perfect but beats burning through tons of solvent, though my next investment is a proper soxhlet extractor.

morganbw - 23-2-2020 at 15:23

I have done a bit of kitchen chemistry myself.
Eventually I will get around to doing a pepper extraction myself.

Syn the Sizer - 23-2-2020 at 17:09

The way I see it is, I was using isopropyl alcohol which if I breath a few fumes will not kill me. Plus I was proving to myself nothing was escaping with a "water trap" not to catch the vapours but just so I could see if vapours were leaving. It was a time consuming process compared to a proper extractor but it did the trick. I haven't weighed the product but I got way more than I expected.

Tsjerk - 24-2-2020 at 02:32

Nice work! How does your extract look? What color and is it crystalline? Did you use black pepper?

Syn the Sizer - 24-2-2020 at 16:07

Quote: Originally posted by Tsjerk

Nice work! How does your extract look? What color and is it crystalline? Did you use black pepper?

Thanks, I wasn't sure if it would work, but was please with how well it did.

Yep, I used black pepper, I didn't have any white on hand. I plan on doing an extraction with white pepper when I get my soxhlet extractor. to compare the products.

I was an idiot and didn't take a pic of the extraction solution or the crude product, posting it was an after thought, oops. The solution was very black, and the crude product was yellow with a faint orange hue. I have recrystallized it and and it is still in the crystallization solution. I will take photos and post the rest, in hindsight I should have waited and posted it all at once. I have a lab report to finish tonight but if I get a chance I plan on filtering it again. Its chilling in a safe location, covered outside in the cold.

I will try and get a good macro shot of the product.

brubei - 25-2-2020 at 04:19

yield?

Amos - 25-2-2020 at 07:06

I'm guessing from your setup you performed multiple extractions by distilling isopropanol directly to your sample and then recycled back the collected extract to the round-bottom? If you have a second condenser you can forget the trap and instead just attach that to the second arm of your receiving flask. Looks like a good way to get by with no Soxhlet though, now for the hard part: getting some decent-looking crystals in high yield.

Syn the Sizer - 25-2-2020 at 15:31

Quote: Originally posted by brubei

yield?

This was just qualitative run, I never intended to post it originally so I am not 100% sure of the yield of the crude product but I will definitely post the details of the recrystallized product. I am expecting to have time to do that today.

[Edited on 25-2-2020 by Syn the Sizer]

Syn the Sizer - 25-2-2020 at 15:40

Quote: Originally posted by Amos

I'm guessing from your setup you performed multiple extractions by distilling isopropanol directly to your sample and then recycled back the collected extract to the round-bottom?

Yep, it was a little more labour intensive than soxhlet extraction but was worth it to recycle the alcohol.

Quote: Originally posted by Amos

If you have a second condenser you can forget the trap and instead just attach that to the second arm of your receiving flask.

I was considering that but I felt that sine it was a sep funnel and not pressure equalized I thought I might run into some issues (unless I misunderstood what you meant).

Quote: Originally posted by Amos

Looks like a good way to get by with no Soxhlet though, now for the hard part: getting some decent-looking crystals in high yield.

It worked quite well in place of a soxhlet extractor. I was considering doing another quantitative run before getting my soxhlet extractor and do a comparison between the real thing and my hillbilly setup.

Syn the Sizer - 25-2-2020 at 19:36

I finally got the solution filtered and the product is now dry and weighed. The yield was 0.22g, but is not very crystalline. I will attach some photos.

Edit: I need to get a better camera or try playing around with settings on this one.

[Edited on 26-2-2020 by Syn the Sizer]

Tsjerk - 26-2-2020 at 03:18

How much pepper did you use?

Syn the Sizer - 26-2-2020 at 16:43

Quote: Originally posted by Tsjerk

How much pepper did you use?

it was about 45g of black pepper.

theoretical yield if it was 7% piperine would be 3.15g of piperine.

0.22g/3.15g*100= 6.98% yield, not the greatest yield.

if you like I could write up my procedure and post it.

Syn the Sizer - 28-2-2020 at 12:50

since it is going to be a bit before I get my soxhlet extractor I am going to do another run using 100.0g of fresh ground white pepper, I am going to assume a piperine concentration of 7% (5+10/2 with slight deflation) for 7g of piperine as my theoretical yield. I am going to post it in a new thread with proper procedure in report format.

Edit: I was unsatisfied with my last recrystallization so I decided to do another one. I did an extraction a month ago just using beakers and lots of solvent and it turned out way better, light yellow and crystalline and I want my current product to look like that.

[Edited on 28-2-2020 by Syn the Sizer]

morganbw - 28-2-2020 at 16:09

You probably have but just in case you have not.
ChemPlayer produced a video using microwave extraction. It looked pretty sloppy to my dumb ass but he/they seemed to get more product than you are getting.
He/they used to have a youtube channel but were too mischievous and had to leave.
You can find the ChemPlayer videos on bitchute. He/they have contributed a lot to the community.

Check out what is presented there, I do believe the extraction presented there will give better results versus what you are pursuing.

[Edited on 2/29/2020 by morganbw]

Syn the Sizer - 28-2-2020 at 20:44

Quote: Originally posted by morganbw

You probably have but just in case you have not.
ChemPlayer produced a video using microwave extraction. It looked pretty sloppy to my dumb ass but he/they seemed to get more product than you are getting.
He/they used to have a youtube channel but were too mischievous and had to leave.
You can find the ChemPlayer videos on bitchute. He/they have contributed a lot to the community.

Check out what is presented there, I do believe the extraction presented there will give better results versus what you are pursuing.

[Edited on 2/29/2020 by morganbw]

I definitely did see that video, I did a similar method my very first extraction using a hotplate to heat the solvent, it worked good but I think I just didn't let mine run long enough as well as after dissolving for the 2nd recrystallization I realized there was still pepper solids in the product.