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Thread: The Black Pepper Tincture Thread, Free Medicine :)

  1. #41
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    It's really hard to tell completely what's going on here. I'm just waiting on drying to see whether I'm getting crystals or just a brown stain.
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  2. #42
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    So.... I failed. I'm not sure what went wrong but I didn't get any piperine. I thought I was going to get it, the colour looked right but it all evaporated into basically nothing. No idea what I did wrong. Maybe I should have left it longer to clump up as you did.

    Ill try again but I'm scared of failure. I get so depressed when lab stuff goes to shit lol.
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  3. #43
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    Quote Originally Posted by elixirmixer View Post
    So.... I failed. I'm not sure what went wrong but I didn't get any piperine. I thought I was going to get it, the colour looked right but it all evaporated into basically nothing. No idea what I did wrong. Maybe I should have left it longer to clump up as you did.

    Ill try again but I'm scared of failure. I get so depressed when lab stuff goes to shit lol.
    I'll have to read over your notes again when I get some time later. I collected the piperine first by catching it in a filter (after sitting for two days). I wasn't going to allow that long for the cedar sample. I just did a couple CCs to see if it milked up. You might need more water, but you should definitely notice it start to settle and separate on it's own before filtering, otherwise the particles will probably be too small and pass through the filter (unless you have one of those fritted glass things. I don't). I washed it further from there instead of trying to purify straight out of the box.

    My rectified piperine is starting to crystallize nicely (after frickin days) but there's still a couple mL of alc solvent in the glass, so I'm going to let it go till it's done. I have a pretty good little crystal going on it from the clump, almost a mm in diameter.

    Extraction of the cloud from the solution is something I plan to look into further. I'm brewing up about 200mL of tincture by adding a little pepper to it at a time and letting it sit for days, with shaking, until it goes dark. Hopefully I can get a gram or two out. Since I'm purifying with alc it might be interesting to distill off the alm/Mercury, redissolve the separated piperine in that, and they dry to get the crystals while at the same time collecting the black Sulphur. The water extraction is still my focus though.

  4. #44
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    I'm going to give it another go. I seriously cannot comprehend where the piperine went!! Could it possible volatize with the alcohol?

    No idea but I'm so pissed that I have to try it again. I will take it slower And allow for clumping and settling as you suggest. The curcumin came out okay. Its not a crystal but a powder. I had a mad tumeric and pepper rice yesterday and it did wonders. I was suffering from inflamed gallstones which really hurt and rverytime I eat something made them worse, but then I ate the rice thinking that it could hurt or it might take down the inflammation and lo' and behold, fixed me right up. Go piperine!!
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  5. #45
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    Right on. Just wanted to make sure that I let you know the piper was in fact filtered off, and it looks like kind of a shaggy powder until you look at it real close. The original crystals were super tiny, like little hairs. I just blew them up so they could be seen better. When I get the big batch going I might see if there is something I can do to tease them out, like maybe distilling off the eth from the solution or just popping the mixture in the fridge for the night.

    After what you said, I definitely believe that you have to get the piperine away from the solution first before you try to do anything with it. When I redisolved in eth it took a lot of stirring and it didn't want to get ate up in solution, but then half of the new mixture had to evaporate before I put put a crystal seed in without having it completely dissolve a couple hours later.

    The recrystallization is going well. I dropped the orange/yellow clump in a filter paper and eyedroppered a couple CCs distilled water over it. Just enough to soak the pile and drive off any water solubles. Then transferred to a shot glass and added a little eth, swish around, repeat, until most of the solid dissolved. The transferred the new dissolved piperine to this glass and let the eth evaporate off over the last few days, nice and slow. This is the result:



    The crystals are much larger and visible without squinting. They can probably get bigger if I had more material, but they are quite pretty. I'm going to dry a couple and then add some heat to watch them melt, which should happen with a minimal amount of heat from my torch under a spoon or something. They're supposed to melt at 129C according to the report I read about the typical chemical extraction/synthesis, so melting into a little pool of waxy will confirm that this is indeed piperine, as there isn't much else it could be at this point.

  6. #46
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    That was cool. I took one of the little crystals and heated it. It melts like ice, going straight to runny and started to boil. I think it decomposed because it solidified as a gum/resin, which I scraped off the spoon with a knife and rolled into a tiny yellow bead with my fingers. I don't think it's a good idea to flux this one.

  7. #47
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    Yes there is no boiling point, only decomposition, and yes, those crystals your growing certainly look exactly like what piperine should look like so I would call that quite a success.

    I understand how you went about it, I just tryed it slightly differently with complete failure so this time I will stick to the plan and see how we go.

    Because I suffer from gall stones and because this really does the trick, its in my best interest to master this one.

    Did you at any stage evaporate off your alcohols or did you simply, add water, allow to clump, then filter. Did you put it in the fridge? How long should heating be do you think? I had mine on a good heat but not enough to boil for about an hour or so, I'm thinking this may be a bit too much. I might skip heating all together and just be much more patient, wait for clumping ect.

    I wish I was a better chemist. If I fail again it will break me lol
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  8. #48
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    I didn't do any special preparation for the clumps in the original images. The tincture was done in a dark place for about 5 days with 70% eth alcohol (grain alcohol diluted with distilled water). Water was added to make it milky, and I believe the "milk" sat for about 48 hours before filtering through coffee filters. I collected the mass in the paper, and that was fairly pure piperine with some oil and I believe a little of the gum mixed in. The recrystallization took even longer, and if I had to guess, halfed the yield. I'll weigh them when they dry off all the way, even though I already swiped a couple of the smaller crystals, just to see how much I lost through purification/recrystallization in alcohol.

    I think an absolute alcohol will work fine. If I figure out how to clump everything better, I'll post it.

  9. #49
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    Okay let's get this straight though, you used about a 4 parts water 1 part tincture? Is that right?
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  10. #50
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    Quote Originally Posted by elixirmixer View Post
    Okay let's get this straight though, you used about a 4 parts water 1 part tincture? Is that right?
    Pretty sure that's how it went down. I didn't measure beforehand. Just added water slowly, letting the milk settle under the remaining tincture. All the light solution sank under the alcoholic tincture, and I added until the tincture layer disappeared. Guessing from looking at it, I suspect 4:1 or 5:1.

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