DOS harmal TEK: IMPROVED HARMALA ALKALOIDS EXTRACTION FROM SYRIAN RUE WITH A/B CLEANUP TO HARMALINE FURMERATE: by: director

of sound 2010 www.mycotopia.net and www.dmt-nexus.com First I would like to outline the procedure. it is rather simple and does not re quire the use of labratory equipment or expensive hard to get chemicals. most pa rts can be modified to work with what you have. lye can be substituted with pota ssium hydroxide and even sodium or calcium carbonate. the alcohols used in the e xtractions can be changed around, isopropyl (rubbing alcohol, ISO-HEET), methyl (HEET, laqure thinner), ethyl (everclear) will all work. i used britta filtered water. you can use bottled, distilled or whatever you have. tap water shouldn't hurt the yeild very much and rue seeds are cheap so you wont notice the .4g loss from using tap water when you are extracting 200g of seeds. the amounts of base used are crucial, too much and some of your alkaloids could be destroyed, too l ittle and they wont crash out of solution. so as a rule of thumb it is a 4:10 ra tio. if you have 10g of seeds use 4g of base, 100g seeds/40g base and so on. usu ally a 50% solution (allmost saturated) does the trick. just add untill the colo r changes. this might be a little more work than a manske extraction but you don t have to deal with salt contamination and the yields and results are clearly be tter. you get much cleaner crystals and not the 'sparkeling dirt' type stuff fro m a manske extraction. you will be able to eliminate all traces of Vasicine and Vasicinone, the more toxic alkaloids found in the seeds most likley responsable for nausia. they are also uterotoxic and a abortifacient so pregnant women or th ose planing on becoming pregnant cannot consume a full spectrum extract containi ng these (not that pregnant women should consume psychedelics and other drugs an yway IMO) the first portion deals with extracting the major alkaloids from the seeds by ch anging them into a water soluable salt form instead of the tannate salt so they can be removed from the seeds by filtration later. for this you will use alcohol , vinegar, and a microwave (crock pot for larger ammounts). as with all extracti ons 3 is the magic number so you will boil the seeds with three fresh portions o f vinegar alcohol. the ammount is not totally crucial as water can hold quite al ot of harmala salts ( 5g/25ml). the second portion comes after you cool and filt er the extracted harmal 'tea'. in this phase you will force the alkaloids out of the water by turniung them into a freebase leaving behind the tannins, chlorofi l, sugars and most of the impurities you dont want in your final product. as you taise the ph you can do it in one shot (which i will do for ease of posting) or follow something allong the line of what the harmal master phlux does. ie the t elepahtine tek., raise the ph to 7.7 and just harmine will precip, push it highe r after filtering out the harmine and harmaline will precip. it also will greatl y reduce the size of material you have to work from 1lb of seeds and a few gallo ns of 'tea' to what you can fit in a 500ml beaker (or 20oz bottle or two). for t his you want to make the tea as polar as possable to reduce the ammount of alkal oids still stuck in the water. you will use lye to do this. and now the magic st arts, as you add the lye nothing will happen at first. just give it a few good s tirs and sit back, the color will change then crystals of the freebase harmala a lkaloids will start to form. these you filter out and desolve in alcohol with vi negar to turn them back into a salt. evapuration yeilds good clean is crystals t hat are good as is. you could stop here if you like but i suggest proceding with the A/B purification. you will have a much cleaner and better looking product. this is where a little more science comes into play. you would scrape up the pow der and re base it and extract the alkaloids with a non polar solvent like tolue ne, xylene or methylene chloride. you now left the salt and sodium acetate and o ther gunk that contaminated your crystals behind in the water solution. now you are at your last step. once you have you alkaloid laden solvent you simply shake it with an acidic solution. i use fumaric acid here as it would go better with your fumarate spice you made and makes some beautiful crystals... there is a gli tch here, fumaric acid does not dissolve well in water but dissolves in acetone

. The consistan cy of fine coffee grinds with a few whole seeds will be fine. the exception is the last (third) acid pu ll mix your vinegar/alcohol mix 50/50 with water or use 50/50 water and vinegar. pick out the rocks and dirt clods. so all this tea you made contains cheifly harmaline. toluene. It takes a while so vacuum filtration is the best. Let it cool and squeeze out the tea. Ayurvedic medicine and a dye. they grind easier) 1. More may need to be added as the seeds absorb the mix. I had a total of 557g (guess they gave me a little extra). For larger a mmounts use a crock pot. BUT the harmaline fumarate does not dissolve in acetone or MEK (if they are dry) so a mix has to be made. THE EXTRACTION OF HARMALA ALKALOIDS: Chems: Materials: syrian rue seeds suitable sized containers for mixing and storing fluids (glass or plastic as long as the toluene dosent dissolve it) Water large plastic spoon for stirring vinegar evap dishes isopropyl alcohol (91% or better) cotton balls. all parts of syrian rue contain alkaloids but most are consentrated in the seeds which can contain up to 5-9%! That would mean there are 50-90g of alkaloi ds per 1 kilogram.05% range. now on to the seeds and the extraction.and MEK. If the seeds a re uniformly moist it will allow the solution to come to an equlibrium inside an d outside the seeds faster once you add an acid/alcohol mix allowing a more effi cent extraction. Stir it every couple of minutes untill it starts to simmer. stems ans sand/rocks could be mixed with your seeds.. Leaves. when harmine is heated in an alcoholic solution of acetic acid it is hydrolyzed into harmaline. you would use 50% MEK/acetone 25% water and 2 5% alhohol for this. about 5-6% of that is harmine and the rest harmaline. or methylene chloride (DCM) 2 leter bottle for filtering fumaric acid Methyl ethyl ketone (MEK) acetone lye or potassium hydroxide (note: put your seeds in the freezer the night before. dont worry about the leaves and stems. witch craft dream en hancer to a noxcious weed as well as a psychedelic incense. some organ ic dyes and tannins as well as several other slightly toxic alkaloids (though in the . surian rue (Peganum Harmala) has been us ed for centuries and has many uses ranging from an admixture to Ayahausca and Ya ge to a middle eastern spice.) Add your alcohol/vinegar mix it is just a 50/50 mix of rubbing alcohol and d istilled white vinegar with enough to cover the seeds with about 1 inch of fluid . The total volume should be just over 3L. Filtering will still have to be done after straining out the seeds with an old shirt.) Now that you have everthing togather and some time on your hands take the se eds out of the freezer and begin grinding. you may need to heat it to get a saturated solution and its okay of you put an excess of fumaric acid in because you will re-crystal your p roduct. 2. After you are done wheigh em out (or just guestimate if it said on the package) do this now becaus e they soon will be a wet mush you cant weigh. ie a few hunderd ppm) now that you have all 3 extractions. If you do that microwave in 45 sec intervals u ntill it is boiling and let it cool before squeezing out the 'tea'. A han . Just load up the seed paste add vinegar/alcohol and set to high. of very hot (not boili ng) water is added per 500g to make a paste and start the saturation of the seed s so osmosis will work better later on when the vinegar is added. You want to grind the seeds as fine as possable. . The best final filter i found was a cotton ball stuffed in the neck of a 2 leter with ho les drilled in the cap. green brillo/scouring pad and ot her filtering materials xylene. there i s a way to compleatly eliminate the harmine and i will explane that later. My total was 500ml of each so 1L total solution. Then stir it a bit more but keep it simmering for 30 min. comb ine them and filter untill clear or let sit over night for plant particals and f ine tannins to fall out. a truely vercatile p lant. For both methods do this 3 times. If it is a smaller ammount of seeds you can use microw ave safe dishes in the microwave. once the seeds are ground 18oz.

Dissolve the salts in the mi nimum ammount of hot abs. Pull this off 3 times with just a litt le xylene/toluene/methylene chloride. When you look at it in the morning there will be a layer of brown 'oil' on the top of a clear milky li quid. There may sti ll be bits of plant material or other gunk you dont want. Its clear for the moment but soon it will start to cloud up.. the stuff in say GNC or store b rand activated charcoal pills is way fine and goes through a cotton ball if you use any pressure or vacuum.. 91% or better). For this i used c otton ball stuffed in the neck of a coke bottle and let it drip dry overnight be fore proceding to the next step. Any lef t over salts will not dissolve and can be filtered out. Once again mix up your lye solution but chill it in the f reezer before adding to your solution. Add your xylene. a small ammount of sal t was added (10g) and shaken causing the entire 250ml or so to solidify into one crystaline mass.6g of this GNC charcoal and f ound out the hard way... If you use something fine let it settle overnight and dec ant/syphon off the charcoal and sediment before filtering. A few more ml of base was added and stired up again to maximize the base to see if anythine else precips out. It ended up taking me several hours to filter the solution but I was rewarded wath a crystal clear da rk neon yellow solution. Charge your flask with t his solution and add acetone some to not quite double the solution but mabey 2530% more. Filter it one more tim e through a cotton ball and pour it in a dish to evap. let it warm to room temp and swirl it around every now ans then untill no more color c hange happens and then then put in the freezer overnight. Not everything will dissolve. Mix up your lye solution in about 3 cups of ice cold wate r and wait for it to cool before adding to the 'tea'. Before you filter you cou ld add activated charcoal if you want to clean it up a bit more if you are going to skip the A/B cleanup.. Set some aside as the acetate salts can be smoked but the furmerate cannot. The filter cake was washed with a little hot vinegar to get out the last little bits of harmaline before it got discarded. I layered in the neck of a 2L first t he cotton ball wetted with a little of the solution then 1/2 inch of sand follow ed by the green scouring pad material cut to size. Keep a dding untill nothing else dissolves.d vacuum pump can be had at amercian science and surplus for under $20. isopropal alcohol ( anhydrous. I added 2. drip only. You will see a color change again. I ended up using 200ml of a 50% NaOH solution. as you . The acetate salt on the other hand is qui te smooth with no burn and barley any taste at all. FREEBASING THE ALKALOIDS: 3. 4. you dont need to use half a gallon. On ce it has all settled decant what you can and filter the rest. Over the next fe w minutes you can watch freebase harmaline crystals form and sink to the bottom. Stir it up real good. mine had straight vinegar added to it. All in a ll you want the 'tea' to be crystal clear. toluene or methylene chloride now (or a mix there of) . the excess vinegar was removed by vacuum filtration. The ev ap goes faster if you use alcohol. an aditional clean up was preformed after the evap by taking the thick yellow/red syrup/crys tals (no not harmaline red. weigh them out and jot that down somewhere.) Now that you have your crystal clear 'tea' you make the alks crash out by ad ding the lye solution.) With your scraped up harmaline acetate salts in hand. Use a course charcoal. This will keep the freebase dissolved rather than letting it crash out when you add the lye. The fumerate salt decomposes into freebase harmaline and malei c anhydride when heated which is about as corrosive as phosphoric acid and you d ont want that going into your lungs.) and re basing them followed by 3 washes with a we ak sodium carbonate (ph5) solution then again suspended in alcohol with vinegar added dropwise untill a semi clear solution was acheaved. I followed by pouring through a perminant coffee filter fitted with a activated charcoal filter to catch any sand that got through.) Suspend your freebase harmaline 'muck' in alcohol (about 20ml/1 heaping tbsp muck) the 'muck' will not dissolve in the alcohol you need to salt it to get it to dissolve so begin adding vinegar untill all the solids are dissolved. You will see a slight color change from a yellowish borwn to a darker chocolate brow n.. I t will pull out the harmaline freebase and leave behing all the salts and the la st of the gunk that was in the alkaloids. A/B CLEANUP / EXTRACTION: 5.

It will be less yellow or not yellow at all your solvent should now be clear to slightly yellow again. . RE-CRYSTAL: 7. Now just evap wh at you have. and as allways be responsable and dont ove r do it. scrape everthing up and again dissolve in t he absolute minimum of cold abs. Filter out t he stuff that dosent dissolve and put back in a clean evap tray. Fast or stick to the diet when using MAOI's.) As you can see the crystals fron the last evap dont look too good.. isopropyl alcohol (91% or better). It should become slightly cloudy and start to change dark yellow-redish. Be careful with these.) Now take some hot isopropyl alcohol and dissolve as much fumaric acid in it as possable. The yellow color will go into the bottom layer. brown and red-orange with a few needles her e and there. In this step you left behind the oily toxic alkaloid s that cause the nausia and gastrointestional problems encountered when eating s eeds or a tincture. chunky..can see i am working the extract from over 500g of seeds in a 500ml flask. different shades of yellow. 6. f eathery. It should go real quick in front of a fan as the alcohol evaps quic k and pull water with them. Add 250ml of this to your xylene/toluene and shake it up (less for smaller ammounts of seeds of course). You should now have these nice super pure needle li ke amber colored crystals of harmaline furmerate. thats because there is a bit of fumaric acid and sodium fumarate in there contaminating your harmaline. You just got rid of the last of the salts and inert matter that was in your extract. Pull that off and add 1/4 that ammount fres h fumaric acid solution and shake again. y our furmaric acid/alkaloid solution. MAOI's can make yout usual dose of mushrooms seem like you just ate fiv e times the ammount.. An additional r ecrystal can be done from pure water to eliminate the very last little bits of f urmeric acid and other gunk.

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