Harmalas extraction: low yield

[reun]

Hi all,

I have recently performed my first harmalas extraction by following this tek and, unfortunately, I ended up with rather low yields, so I'd like to understand how I can do better next time. In short, I used 100 g of Syrian rue and I got only 500 mg yield out of it, which is 0.5%. I was expecting much more. Any tips on where I could improve next time?

I'll summarise very briefly the steps I followed:

1. Add 100 g of Syrian rue into a container with 500 mL water and then place the container into a freezer
2. After the container freezes, let it thaw out
3. Place the water-rue mixture into a large saucepan, add 30 mL of white vinegar together with about 450 mL of extra water and bring it to near-boiling temperature
4. Simmer the mixture for 20 minutes, top it up with another 50-75 mL water and simmer for 20 more minutes
5. Remove the saucepan from heat and let it cool, then move the water into a large glass container (I used a flask)
6. Slowly add sodium carbonate into the glass container until the mixture stops changing colour and it all looks milky
7. Place the container into the fridge for 3 hours, then decant it by removing 90% of water and topping it back up to 1 L in total -- do this at least 7 times
8. NOTE: it is recommended to remove water into a separate large container which will also accumulate some harmalas, but in theory, skipping this step should still yield 2-3%
9. After performing step 7 multiple times, you should be left with near-clear water at the top and some sediment at the bottom. Decant as much water as possible and place the watery sediment into a separate glass dish, then let it dry out in an oven on low heat
10. Scrape the dry powder off the dish and you are done -- be sure to use gloves here, because harmalas can be absorbed through the skin

I will not skip step 8 next time, but I was still expecting to get much more even with the streamlined process.

Any tips would be highly appreciated!

Many thanks

 

[Sakkadelic]

Hi reun,

Simmer the mixture for 20 minutes, top it up with another 50-75 mL water and simmer for 20 more minutes

Well, you need to do this 5 or 6 times, a 40 min boil isn't enough especially with whole seeds. You then combine the water from all boils and base it. If you haven't done that your low yield is totally expected.

Place the container into the fridge for 3 hours, then decant it by removing 90% of water and topping it back up to 1 L in total -- do this at least 7 times

Repeating this 7 times is excessive and 3 hours wait is not always long enough. I expect some losses here

 

[reun]

Well, you need to do this 5 or 6 times, a 40 min boil isn't enough especially with whole seeds. You then combine the water from all boils and base it. If you haven't done that your low yield is totally expected.

Ah, thank you! This is highly useful information. So, just to make sure I understand, the process is this:

1. After removing the hot saucepan (first round near-boiling), place the water into a separate container, let it cool and follow from step 6 onwards
2. But instead of discarding the seeds, add another 1L of water (no need to freeze them again) and 30 mL of white vinegar and repeat the process 5 times from here

Am I reading this right? My only concern is that I need a lot of water jugs to handle all of that!

Repeating this 7 times is excessive and 3 hours wait is not always long enough. I expect some losses here

Okay, so you think I can stop after about 4-5 times then? I also felt that the water was mostly clear by that stage. And yes, perhaps I could extend 3 hours to 4 or so

So, suppose that I:

1. Repeat the boiling step 5 times
2. Drip the decanting to 5 times but extend the waiting period to 4 hours
3. Capture the discarded water into another vessel and decant it later

I should get close to 4-5 g from about 100 g of Syrian rue, is that right?

 

[doubledog]

I would increase amount of water in first boil.
You should repeat the boils at least 3 times and squeeze water out from seeds in between.

 

[northape]

All these steps are confusing. Extracting harmalas is extremely easy. Cook rue in enough water (30ml / 1g of material) at pH6 or lower for a few hours, then filter and base the solution. After a few hours (or even better overnight), your harmalas will settle at the bottom. Everything else is done simply to purify them.

 

[TransistorBass]

I used the no-filter-TEK you are doing and it worked great, I was really happy with the results though I used Lye as that’s what I had in the house. I’ll have to look for my Yield results, I think I put them in the original no filter TEK thread.

Edit- 5.3% Yield TEK - Speedy No-Filter Harmalas Tek (draft)

 

[Sakkadelic]

Cook rue in enough water (30ml / 1g of material) at pH6 or lower for a few hours, then filter and base the solution.

Base first, decant and wash, then acidify and filter for easier filtration.

 

[reun]

I used the no-filter-TEK you are doing and it worked great, I was really happy with the results though I used Lye as that’s what I had in the house. I’ll have to look for my Yield results, I think I put them in the original no filter TEK thread.

Edit- 5.3% Yield TEK - Speedy No-Filter Harmalas Tek (draft)

Thanks for the link! A part of your this tek caught my attention:

Note: A 3rd simmering step is perfectly fine to do, but will increase the volume of water making this no-reduce tek more difficult. Even the 2nd simmering step is optional. If you prefer to only work with a small amount of liquid and still get a 2-3% yield, just do the first 40 minutes simmer.

So, this is saying that even if I simmer only once, I should still get about 2-3 g out of 100 g of Syrian rue, but I only got 500 mg. That's the mystery and I'm still not entirely sure what I did wrong! As far as I'm aware, I pretty much followed this exact tek

 

[reun]

Base first, decant and wash, then acidify and filter for easier filtration.

Hm, the tek I followed seems to apply this in a different order. Simmer in vinegar (acid), then basify (sodium carbonate), and then decant and wash. Let me know if you have any particular tek in mind

 

[TransistorBass]

Thanks for the link! A part of your this tek caught my attention:

So, this is saying that even if I simmer only once, I should still get about 2-3 g out of 100 g of Syrian rue, but I only got 500 mg. That's the mystery and I'm still not entirely sure what I did wrong! As far as I'm aware, I pretty much followed this exact tek

From what I remember I did the whole TEK with all the simmers, and the recovery of the sediment in the rinse water.
There is always the chance you have some less giving Seeds.

 

[The Sofa Traveler]

Low yield can also come from bad or weak seeds. Once, I had seeds with absolutely no harmalas in them. Imagine my surprise seeing no precipitation while pouring the SC solution over the filtered soup. When I checked the remaining bag from the same batch, I noticed it had a strong musty smell. Vendor was probably storing them in inappropriate conditions. I also had lower yields from old seeds (>1 year) but fresh seeds most often yield about 5%.

 

[reun]

Alright, thank you all for contributing to this discussion. Just a quick update that I'm running another extraction now, I should wrap this up in a few days, at which point I will report my yield results, and we'll see whether my corrections have helped, but even before I get to this stage, I have discovered something unexpected, which I documented in this thread. In short, some rock-like sediment formed at the bottom of my vessel, and even though I removed it, I feel like it absorbed some of the harmalas that were sitting at the bottom, so I was trying to figure out what it was and how to prevent it from happening again.

On a separate note, just wanted to report that I had my first mild harmalas experience today. I took 110 mg, initially I didn't think it was working at all, but sure enough, about 90 minutes later, I was in a deeply relaxed state. I found it interesting how harmalas can completely shut down your internal dialogue and leave you sitting in a peaceful, relaxed state. I also felt that harmalas work as highly potent anti-anxiety agents. And I felt zero nausea or any negative reactions, really. That said, I don't see myself taking 110 mg again -- I do see myself microdosing on about ~ 50 mg or so from time to time, but for a proper experience, I will definitely be upping this dose to 200-250 mg.

 

[reun]

Alright, a quick update! I ran another extraction with a few corrections along the way and this time I had a really solid yield. I used 70 g of Syrian rue and I ended up with 3.85 g, which is 5.5% -- I'm very happy with that! Thanks everyone for helping me make those corrections!

 

[Ra-Horakhty]

Alright, a quick update! I ran another extraction with a few corrections along the way and this time I had a really solid yield. I used 70 g of Syrian rue and I ended up with 3.85 g, which is 5.5% -- I'm very happy with that! Thanks everyone for helping me make those corrections!

Amazing, I was going to ask you how it went, it seems like it's a success.

Could you explain the steps and corrections you followed this time, it would be great

 

[reun]

Could you explain the steps and corrections you followed this time, it would be great

Sure!

The process is very simple:

1. I left 70 g (but I'm pretty sure it would work just as well with 100 g) of rue in 500 mL of water inside the freezer overnight and then let it thaw out
2. Place the thawed rue-water mixture into a saucepan and add another 500 mL water plus 30 mL white vinegar
3. Bring to near-boil and simmer. Admittedly, I allowed it to boil for a bit (just didn't keep my eyes on it enough) -- I believe this is discouraged but not catastrophic
4. Simmer for 20 minutes, then add half a cup of water and another 15 mL vinegar and simmer for another 20 minutes
5. Remove the saucepan from heat and let it cool. I just left it outside for a few hours
6. Transfer the liquid from the saucepan into a 1L container and add just enough sodium carbonate to turn the entire mixture dark milky, then leave it in the fridge
7. Return to your pot and fill it with another 1L water and 30 mL vinegar and repeat step 3-6 twice more. On the 3rd time squeeze liquid out of seeds as best as you can
8. After finishing step 3, you should have 3 1L containers with harmalas and sodium carbinate mixtures. Leave them in the fridge overnight
9. The next day remove 90% of liquid from all 3 containers into another large container (aim for 6-8L, I used 3 3L containers)
10. Merge the sediment from all 3 of your containers into a single one and fill it back to 1L of water, then leave it in the fridge
11. 4 hours later, empty 90% of the liquid in your harmalas bottle into the large container. Do this at least 3-4 times
12. Note, water should be pretty clear by the end, I simply disposed of the water from the last washing cycle without adding it to my large container
13. Let the large container with all your excess water settle overnight and then dump 90% of the water from it and place it into another 1L container (you can merge with the first one, but you will need to wash it for a bit longer). I've found that my large container had about 40% of all the harmalas
14. If you merged your containers, then you'll find that you have all of your washed harmalas sediment sitting in a puddle of water. Transfer it into a pyrex dish. You can carefully use a turkey baster to remove some excess liquid
15. Place the Pyrex dish into an oven on fan bake at 50-60 degrees celcius and leave it there for a few hours until dry
16. Celebrate

In terms of what's different:

• I think I forgot to add the 15 mL vinegar at the 20 minute mark the first time I did it
• I only did one boil cycle the first time, whereas this time I did 3
• I did not collect water into the large container the first time around
• I did not let the mixture settle overnight the first time around
• Initially I only allowed for 2-3 hours for harmals to settle between washes