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eithan0693

Syrian rue

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PsychoNanoNaut

I am tuned in sir.

Are you gonna use a blacklight to show us how them crystals glow? Will extracting the crystals reduce the amount of stomach discomfort when taking the rue? 

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eithan0693

This is a compilation of many different teks with some improvements made.

If anyone would like to add, or ask questions feel free. I will report yield back when I find the cup for my mg scale. It's on the low side this batch of Syrian rue seeds is almost a year old but the Actives are still active. I will make note that there was much less harmala than harmaline this could be due to degradation. Enough with the intro! Here it is.

****************************************

Materials Required

Source Material:

Syrian Rue (seeds)

Solvents:

Water

Reagents/Desiccants:

Salt (Kosher Salt, Rock Salt, Iodine Free Table Salt)

Vinegar or Citric Acid

Sodium Bicarbonate/carbonate

ammonia carbonate

Rubbing alcohol

Equipment:

2 Funnels

2 Big Collection Jars( minimum )

Coffee Filters( highest grade )

Cotton Balls( polyethylene stuffing ; New clean pillow stuffing )

1 Large Pot ( stainless steel or glass )

1 Small Pot

1 Metal Screen / Strainer

Syringes

active coal

Zinc dust

Magnetic stir plate ( optional )

Pyrex glass oven dish

Part-1

Step 1- Boil Seeds

Boil the seeds in 1000ml 5% acetic acid. It usually takes about 45 minutes.

Tip: Let the seeds settle for awhile before pouring the liquid out of the pot.

Use whole seeds to reduce the amount of filtration needed.

Step 3 - Clean Brew

**filter until nearly clear solution, more or less filtering may be required, filter less at own discretion and at the chance of purity contamination**

You want to begin filtering your solution through a metal strainer. You'll want to add the solids back into the pot with fresh acid and continue boiling while you filter the rest.

Next you will want to pack VERY loose cotton balls into a funnel. You want enough so that the cotton won't go through the hole when you add the liquid, but not enough to restrict the flow much.

These first few filter passes take the longest because of the sludge in rue. When the first funnel gets clogged, decant the remaining liquid out and add it to the second collection jar until it gets clogged.

Once it passes through the tightest cotton easily, move onto coffee filters and do the same process. If one gets clogged, move it to the other funnel. It's a real pain to get rue filtered properly but it's worth it for pure product.

Important:  Before you base the brew you want it as clean as possible. If it cannot be filtered easily through a coffee filter, it is NOT ready. If all of that extra gunk is not removed, it makes it almost impossible to retrieve the alkaloids once they are freebased. Take the time to clean your brew and you will be rewarded later.

Step 4 - Reduce

Once you have the solution filtered, you can reduce it. Take note of the volume of the solution and reduce to 500ml for each pull, 1500ml total, if it's not already reduced from the simmer

Step 5 - Base

After you have boiled, reduced and cleaned at least 3 pulls/boils you want to perform the first freebase of the molecules. Before you base the brew, run it through a coffee filter one more time just to make sure it is as clean as possible.

After you have filtered the brew, make a sodium carbonate solution by taking 10 grams of sodium carbonate and adding as much cold water as needed(~120mL) and mixing until dissolved.

Once you make a basic solution you'll want to add it slowly to your tea while stirring.

Keep adding it slowing while continuing to stir and you'll see the color changes starting to take place. You may have to make more basic water. Keep adding the base solution until everything goes milky, then add a little more to be on the safe side.

That milky color is your alkaloids precipitating out.

Wait one hour for solution to separate, the percipitate is your harmalines

Once your alks have settled, you want to decant and filter as much of the basic liquid as possible

After you have decanted or filtered the basic (high ph) water off the top, you want to add 10ml at a time of hot vinegar then water into your funnel alternatively until your freebase alks redissolve back into the solution as harmala acetates. Once your alkaloids are redissolved, filter out anything that won't dissolve. This is mostly plant matter and oils. ( use only as little liquid as will dissolve the alkaloids )

Step 6 - Manske

Once you have redissolved your alkaloids in a minimal amount of fresh, hot vinegar and then filtered the solution, it's time to perform the manske.

There are four ways you can perform the manske.

The first and the "official" way is:

Recommended

Take a note of how many ml's you have and add 10 grams salt per 100ml solution. Make sure your solution is hot before you add the salt, otherwise the harmalas might fall out too soon. Allow to cool slowly.

(12+ hours)

The second way by Phlux-:

Prettier Crystals

Take note of how many ml's you have and saturate the same amount of fresh distilled water with salt. Add them together and allow to cool slowly. This seems to work better with an excess of water/vinegar to allow the crystals more room to grow.

(12+hours)

The third way:

Completely saturate the solution with salt ( 20 grams of salt/100ml of distilled water )and allow to cool.

Not Recommended for Final Manske due to the higher chance of more salt contamination. It's better to use one of the above methods, preferably Phlux's on the final manske and push any remaining alks out by reducing the solution further after you filter the harmala hcl.

(12+ hours)

My way- reduce solution to 100ml and measure 300ml more of distilled water. Add 100ml of water to solution. Mix 40 grams of salt into the remaining 200ml of water then add saline water to solution. Stir well let cool to room temperature and place into a fridge. This process works well at forming filterable crystals within 6 hours. Can be used for all 3 salt outs.

Step 7 - Filter

Once you are confident that no more growth is taking place, filter the solution with a coffee filter to collect all of the crystals.

This produces a stable usable 80%+ pure product of harmala and harmaline.

Part 2 - cleanup of salts and hydrogen reduction

1. Repeat Manske untill you have clear crystals. Mostly it needs about three times. Sometimes the tea is so concentrated that the crystals don't become much cleaner.

2. In the last Manske, keep the crystals in the filter and clean your recieving vessel or take a new one. Then slowly drop cold water into the filter until all the crystals have dissolved. This can be a lot of water, 2-4+ cups. Save this water.

3. Bring the water with the alks to a boil and add a bit of active coal. Keep stirring for about half an hour. Put it on a lower heat so it's just under boiling and let the charcoal sink to the bottom (when boiling it won't sink and charcoal can be hard to filter). Then slowly pour off through a filter.

4. Bring the filtered solution to a boil again. Mix 1 gram of ammonia bicarbonate into 15ml of water. SLOWLY add drops of ammonia to solution while stirring in between each drop. At a certain point small clear needle like crystals will appear on top of the solution. You will NOT need the full 15ml of ammonia yet, Don't add more ammonia but keep stirring slowly for at least 30 minutes. This will precipitate most of the Harmine. Filter the solution and save your Harmine.

5. Add a bit more of ammonia(1-5 drops) to get another fraction which will be mostly Harmaline with some Harmine. Filter and save alks.

**harmala likes to float, harmaline likes to sink and is much darker is colour**

6. Now you can take your solution from the heat and add more ammonia till all alks crash out, wait 30 minutes for this to finish. This will be mostly Harmaline. Under a mic you can clearly see the difference with the Harmine. The Harmaline freebase looks pinkish brown and makes flat crystals while the Harmine is needle-like and clear. Filter and save your Harmaline.

Step 8 - hydrogen reduction

1) -Mix 1 gram of Harmaline into 75ml of Vinegar

2) -Add 3 grams of Zinc Dust (not Zinc Oxide, only pure Zinc Dust)

3) -Mix Zinc around and release any gas (Hydrogen gas DOES form, be careful)

Magnetic stir plate optional

After 1 hour add another 25ml of vinegar and 1 gram of zinc

Total of 100ml of vinegar and 4 grams of zinc

4) -Wait 10 more minutes and Filter out the remaining Zinc Dust from your Harmala Vinegar solution.

5) -Add Sodium Carbonate Solution to the Harmala Vinegar solution until there is no more color change/ ph of 8.6 .

6)Wait 2 Hours and filter solution to recover most of the TetraHydroHarmine (THH)

7)Dissolve your THH into 99% Isopropyl Alcohol and wash previous collection jar with this alcohol, filter and discard any solids, these are Zinc Carbonate leftovers. Evaporate the alcohol to leave clean THH!!

** THH precipitates out at ph=8.5

**harmala precipitates out at 8.6

**harmaline precipitates out between 9-12

** THH should also "glow blue green" when added to a smidgen of water and painted onto glass under a blacklight like acid.

** Harmaline glows green under a blacklight when added to a bit of water and smudged onto a glass surface and held under blacklight.

** decant - to syphon off the liquid leaving the precipitate at the bottom.

**Sodium carbonate from sodium bicarbonate. Bake the soda at 400°F(200°C) for 30 minutes to 1 hour. The time isn't critical, you can't 'overcook' the soda, but you want to be sure to drive off all the water.

**

Substance PH value

Sodium acetate 8.9

Sodium benzoate 8.0

Sodium bicarbonate 8.4

Sodium carbonate 11.6

Acetic acid 4

**7g of sodium bicarbonate neutralizes 100mL of pure 5% acetic acid to a ph of >7

5% solution of acetic acid, HC2H3O2. Let vinegar be called V.

HC2H3O2 + NaHCO3 ===> NaC2H3O2 + CO2 + H2O

Atomic weights:

Na=23

H=1

C=12

O=16

NaHCO3=84

HC2H3O2=60

100mLV x 5gHC2H3O2/100mLV x 1molHC2H3O2/60gHC2H3O2 x 1molNaHCO3/1molHC2H3O2 x 84gNaHCO3/1molNaHCO3 = 7g NaHCO3

NaC2H3O2 is the salt of a weak acid and a strong base (NaOH) so the pH of a solution will be >7**

**acetic anhydrade possibly is a better option for H2 reduction, research required**

**I've used tap water with only slight decrease in yield

Sent from my personal jungle off of my phone, beware of typos and carnivorous plants

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Mushinist

Looks good, and nice write up.

I just kept mine at full spectrum free base, though I admit the HCl looks better being xtals and all. One of these days I'll get around to separating the three out but in the meantime it works as intended.

It seems I'm pretty sensitive to harmalas, any more than 150mg and I'm purging, by that time I'm walking like I'm drunk with some ridiculous tracers, psychedelic all on its own.

Anyway nice job friend!

 

Peace

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eithan0693

That Is very accurate, most people can stop at the salt out step with no issues. Unless your synthesizing THH from harmaline there's really no point to take it any further. The only impurity after the manske is salt and 1-5% fat content so I wouldn't worry.

As for purging, there's 3 different types of purge, there's sediment purge which is terrible, then there's oh shit I took too much, then there's crap I forgot I ate cheese 6 hours ago and now have serotonin syndrome. Purifying really only helps the sediment sickness.

Sent from my personal jungle off of my phone, beware of typos and carnivorous plants

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eithan0693
I forgot I had replied to this, I'll put some pics of my own to add with yours.

The HCl looked a lot cleaner after the 3rd manske. Pic after that was before, and very dark looking, looks like wet insulation.

Then I converted back to freebase, very light tan almost white harmala freebase.

20160212_080232.jpg

20160208_191159.jpg

20160217_140525.jpg

Very nice work! Thank you for sharing

Sent from my personal jungle off of my phone, beware of typos and carnivorous plants

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Toxic

I got a shit-load from a new source. This extraction is from Afghanistan seeds, whereas the first extraction I ever performed on Peganum harmala was from Indian seeds. I'm finding the Afghanistan source is about 3x more concentrated than the Indian source. Personally, I didn't find that using more than a dash of vinegar makes the extraction more successful.

http://i.imgur.com/8CQrnTe.jpg

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Mushinist

I'll tell you what, I won't make the mistake of grinding the seeds before extracting again, freakin nightmare filtering that sludge.

I have plenty to last me awhile, if I do it again might just do a cold water extraction instead.

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Toxic

I didn't pull anything from the first boil, but I wasn't expecting anything from it just by judging the color of the brew. The lighter, more transparent second and third boils are more useful for extracting... if one has a poppy field or something in their backyard the first steeping is of course useful.

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Toxic

I may try a cold water extraction, but I say "may" because I don't want anything to grow too much. It seems that caapi is more suited for cold extractions, albeit I've never tried a cold water caapi extraction. Even though I have a lot of rue extract, I'm going to be spending another two days doing another extraction so I can have a whole new batch to make some freebase. When smoking harmalas do you use two times less than what you usually use when using it orally? Hopefully that makes sense, because if I'm correct freebase alkaloids are less heavy than their salt/acid form.

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Mushinist

When I make my changa I use a 1:1:1 ratio, harmala's, dmt, herbs. Its harmala "heavy" because I like the effects and the inhibition on the oxidase system smoothing and prolonging the trip some.

As for orally, I can't personally go above 150mg of freebase before the purge happens and I don't care for that, especially while tripping. Some can take it in the 300+mg range with little issue.

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Toxic

If my gram sale is correct, I've used ~200-250 milligrams many times in a day, but didn't trip at all. If I indeed was using that high of a dosage I suspect that my body breaks things downs quickly, because I administered these amounts multiple times in a day and never had a psychedelic experience. However, with that being said, I'm using a salt form, not the freebase form. You may want to dissolve the freebase in some orange juice to turn it into an acid to see if that helps with the stomach issues... because I've never had stomach issues with harmalas - not one bit.

I really need to get a milligram scale.

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Mushinist

I have tried that and its always the same thing. At 150mg I'm getting a drunken feeling and some ridiculously long tracers from it, pretty wild all by itself really.

Everyone is different, so doses on harmala's will vary from person to person, sounds like you have a higher tolerance for it then I do.

Its not as bad if I predose 50mg and then take another 100mg after 30-40min, usually I'm good then.

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Toxic

Has anybody here with the cleaner extract experienced perspiration? I've never bothered to go farther than the first manske, as it seems much analysis by people such as Shulgin show that the salt precipitations are free of the "toxic" alkaloids vasicinone and vasicine, but the books aren't always right.

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Mushinist

I did 3 manske on mine just to be sure, but to answer your question, no I don't experience that.

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eithan0693

So it seems I'm not the only one who's thought about smoking harmalas. I decided to smoke 25mg of thh but had eaten pizza earlier that day, and noticed no negative effects. This was me being forgetful and curious, I really didn't feel a whole lot when smoking it. I prefer orally. I've taken citrines and salts, and freebases up to 250mg in one day. I'm curious about multiple 250mg doses not doing anything that seems like you may need to switch to the teks for mankes with less salt in the end product. Good rule of thumb, if you see square crystals, do the manske again, add less salt and cool slower. What I'm really curious about is noting that tobacco has harmala alkaloids in it , people smoke and eat dairy, do harmalas inhibit the oxidase system or no? Any thoughts?

Sent from my iPhone using Tapatalk

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Toxic

I can tell you that my extract isn't the purest, but I'm fairly sure I was using at least 200mg multiple times in a day. It's not that I don't feel anything, it's just not psychedelic by iteslf for me. However, I'm sure if I took much larger dosages it can become psychedelic. I also say I'm fairly sure because the first time I combined harmalas with mushrooms - which was ~200-250mg of harmalas with 2 grams of mushrooms - it was an overdose and really made me aware of how much the harmalas are working. Thereafter that experience, by naked eye I took an 1/8th of what my scale reads as ~200mg - which I suspect to be about 20-30mg and it was a lot smoother - no worries of a hospital visit at all. The perspiration happens specifically when I combine it with mushrooms. By itself - my body can tolerate harmalas very well, but when combined with other things that I'm more sensitive to - the harmalas become a lot more apparent.

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Mushinist

Yep, for shrooms I don't take more than a 100mg, otherwise it just last too long, but do go good together in the right ratios. If you are taking them regularly then you may have built up a tolerance, but again everones chemistry is different so not sure what's going on with the perspiration thing.

As for the tobacco thing, the harmalas present are probably so minute that it doesn't have an effect, plus I think cigs have other leafs blended in that may not carry any at all. Maybe, not sure though.

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Toxic

I'm not so worried about the perspiration, as this is a specific effect associated with the ingestion of peganum harmala seeds; I'm just wondering if any trace materials in my extract could be causing it, as it also has a bronchodilating property - which is indicative of the "toxic" alkaloids of rue.

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killercub93
On 1/2/2017 at 2:45 PM, eithan0693 said:

Here is from left to right

Harmala free base, and harmala acetate

Harmaline free base, and harmaline acetate

Tetrahydraharmaline free base, and Tetrahydraharmaline acetate

 

Note that dry free bases don't glow.

IMAG7677_1.jpgFor some reason i think this looks so cool!

 

3

 

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Mushinist
4 hours ago, Toxic said:

I'm not so worried about the perspiration, as this is a specific effect associated with the ingestion of peganum harmala seeds; I'm just wondering if any trace materials in my extract could be causing it, as it also has a bronchodilating property - which is indicative of the "toxic" alkaloids of rue.

You could just do another clean up and see if you're still getting the same effects afterwards, yours looks very dark, and mine looked very dark until I cleaned it up and then it was a light shiny gold color (in the pic). Each time it got lighter and lighter so it had to be removing something.

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