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.