Chromatographic Seperation Techniques?

Discussion in 'Harvesting and Processing Marijuana' started by WuShock, Mar 13, 2009.

  1. Anyone familiar with any chromatographic seperatory methods for THC purification? A simple alkane extraction is not enough and I'm curious about how hydrophobic interaction chromatography or reverse phase HPLC will work out. Off the top of my head, I was thinking of maybe trying a phenyl-sepharose or C4 column with a gradient ethanol or methanol elution. Anyone knowledgable in this field?
     
  2. Lol, go for it. I have no idea what you said, but if it works and I can find the ingredients at Rite Aid... I'm in.
     
  3. So are you planning to use chromatography to tell the concentration of thc contained in the bud, or to actually use it at a route of purification? I'm familiar with basic understanding of mass spec/Gas chromatography but I didn't know it could be used for purification.
     
  4. haha....ummm... yea the chromatographic helps the thc purify by extracting it and...umm.

    Hahaha, na i have no clue bro.:D
     
  5. 1) HPLC is semi prep.

    even the biggest, gnarliest Prep columns, that cost 10s of thousands of dollars brand new are only capable of about 10 gram loading,

    in many cases, these even require special pumps, as they should truly be called RHPLC or RIDICULOUSLY high pressure liquid chromatography (yes. high PRESSURE. why do you think it is such high performance?).

    2) Reverse phase is for seperating POLAR compounds. Why?

    i) it is expensive and is avoided at all costs. indeed, people throw away silica, but they reuse c-18. Synthetic chemists often have 1 and only 1 C-18 column for a whole year, and simply run MeCN through it until it is clean.

    ii) the whole point of chromatography is to choose a stationary phase that has LESS affinity than the mobile phase for the analyte.

    if you choose something that is non-polar, like THC, it will have MORE affinity than the mobile phase and it will stick.

    THC dissolves in Aromatics like benzene, toluene, etc and alkanes like Hexanes, pentane, etc.

    reverse phase are typically c-8 to c-18 or possibly aromatic.

    these are the EXACT SAME as the solvents.. thus there are few solvents that are BETTER at dissolving THC than the stationary phase.


    3) the whole issue with THC isolation is that the CBN, CBD and other nameless oligoterpenoids (of which THC is a member) are all very similar in retention factor.

    even a super duper high quality BHO extract, completely clear, golden orange or yellow (which is "close" to clear, vs dark red or opaque) will yield a full un-seperated band on a Prep-TLC plate, no matter the system.

    indeed, an HPLC/GC/etc plot is like peak-peak-peak-peak-peak-peak all in succession, sometimes overlapping (of cannabis)


    if you look in the literature, the best results of high purity THC from extacts are the result of repeated alumina flash columns using typical solvent systems (Chloroform ethyl acetate..)

    this is kind of old, and it seems as though most poeple use silica and DCM instead of the alumina and chloroform.
     
  6. ^^^ Agrees )
     
  7. where is Macgyver when you need him!!??!?
     
  8. Ive done this with a small amount of weed just out of curiosity. Ethanol extraction and separation on a silica column eluting with DCM. Collected several fractions. Assumed the golden viscous oil fraction was THC and related substances - the smell was very distinct. Must make sure you remove all the DCM.
     
  9. what do you guys smoke, out of curiosity?? I am curious as to which strains you scientist's prefer, grow, or tend to smoke. random question, i know.
     
  10. I wish I understood what you guys are talking about..
    I believe my crc column acts as lc column. A very observant operator can pull water clear terp fraction off main pour....
     

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