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What is wrong with the MDMA available today? - v2

user666 said:
Could you ask them whether they are capable of doing some sensitive tests for the presence of low-concentration OH groups in the sample ?
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Following suggestions on here, I asked them for the following:

...
Known inhibitors:
MDDMA [1,2]
MDTMA [2]
1,3-bis (3,4-methylenedioxyphenyl)-2-propanamine [3,4]
N-formyl-1,3-bis (3,4-methylenedioxyphenyl)-prop-2-yl-amine [3,4]

Also particularly interested in M-ALPHA-HMCA [5]

Additionally: bk-MDMA, MDE, ethylone, butylone, 6-MAPB, n-methyl-MDDMA, 3,4-dimethoxyamphetamine and 3,4-dimethoxy-n-methyl-amphetamine, and in general all the regioisomers of MDMA?

Also, 3-MMC, 4-MMC, 5-APB, 5-MAPB, 6-APB, but I see you already listed these.

And some were keen to see NMR, GC/MS MALDI, RAMEN results and anything else that can be thrown at it.

I know I'm asking for a lot so appreciate all that you can do.

Refs:

[1] Optimization of HS-SPME/GC–MS analysis and its use in the profiling of illicit ecstasy tablets (Part 1), Forensic Science International 187 (2009) 73–80
[2] Binding Mode Selection Determines the Action of Ecstasy Homologs at Monoamine Transporters, Mol Pharmacol. 2016 Jan; 89(1): 165–175
[3] Pharmacological Characterization of Ecstasy Synthesis Byproducts with Recombinant Human Monoamine Transporters, JPET 314:346–354, 2005
[4] Synthesis markers in illegally manufactured 3,4-methylenedioxyamphetamine and 3,4-methylenedioxymethamphetamine Int J Leg Med (1993) 106: 19-23
[5] Identification of a new M-ALPHA analog and MDMA in an illegal health product, Forensic Science International, 313 (2020)
....

They just said, yeah we can do that. In retrospect it wasn't the kind of response that makes me feel asking for any more detail would get us anywhere.
 
The prof says that substituted phenethylamines containing the phenolic OH groups can be separated from those without OH groups by using a selective acid-base liquid-liquid extraction procedure on the base oils. This exploits the acidity of the phenolic OH (pKa ≈ 9–11), which allows deprotonation into water-soluble phenoxide salts under alkaline conditions, while non-phenolic amines remain neutral and organic-soluble.
Solvents needed are: Dichloromethane (DCM), Ethyl Acetate, distilled water.
Reagents needed are: 1 M NaOH, 1 M HCl, anhydrous Na₂SO₄.

Interestingly, the phenolic fraction is supposed to fluoresce under UV and stain with FeCl₃.
 
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Well it was a long time ago but I did an acid base extraction according to instructions from @G_Chem. There were two options depending on whether xylene or dcm was used. With xylene it was:

Weigh out 1g MDMA in bottle
Dissolve in 50ml of WATER
Add 50ml of XYLENE
Shake vigorously for 5 mins
Let sit
Remove and discard XYLENE (top layer)
Add another 50ml of XYLENE
Slowly add LYE to mdma/water/xylene solution in increments of 0.5 – 1.0g until pH 12
Water gets cloudy and mdma rises into xylene
Let sit for 1hr, occasionally shaking
Shake for 5 mins
Let sit
Separate XYLENE/MDMA and save
Add 50ml of XYLENE, and repeat above 3
Should now have 100ml xylene and mdma freebase
Mix 5g LYE with 100ml WATER
Let sit until all disolved
Add to XYLENE/MDMA freebase
Mix 3 mins and separate
Discard water layer
Add 100ml WATER to xylene/mdma
Shake for 5 mins and separate
Discard water layer
Repeat above 3
Dilute HCl to 5%
Add 50ml of dilute HCl
Shake for 10 mins
Separate HCL powder solution
Repeat above 3, TWICE
Combine separations and dry on a plate
Disolve in fresh WATER and dry on a plate


Does this look right?

It didn't improve the experience.
 
I will ask the prof for details but IMO you should not attempt it before you have confirmed that your sample really contains compounds with OH groups. Otherwise, it is a waste of product.
 
user666 said:
I will ask the prof for details but IMO you should not attempt it before you have confirmed that your sample really contains compounds with OH groups.
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Ok, is that from a wasting time point of view or are there safety risks applying the procedure without OH groups present?

And is there a practical at home way of testing for the presence of those compounds?
 
ThreePointCircle said:
Ok, is that from a wasting time point of view or are there safety risks applying the procedure without OH groups present?
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More like wasting product. You've already tried the AB extraction.
ThreePointCircle said:
And is there a practical at home way of testing for the presence of those compounds?
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Maybe FeCl₃ staining.
These Kykeon folks should detect it, though.

ThreePointCircle said:
...RAMEN results and anything else that can be thrown at it.
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Raman

Ramen is this ;)
 
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user666 said:
More like wasting product. You've already tried the AB extraction.
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Every time I try a new vendor to see if I can find the unicorn. I have kept a lot of the bad stuff lying around so wasting product isn't a bad deal
user666 said:
Maybe FeCl₃ staining.
These Kykeon folks should detect it, though.
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I've lost faith in Kykeon tbh. Would also take more time and money to arrange.
user666 said:
Raman ;)
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That's an embarassing typo :ROFLMAO:
 
ThreePointCircle said:
Every time I try a new vendor to see if I can find the unicorn. I have kept a lot of the bad stuff lying around so wasting product isn't a bad deal
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I heard that recently Meh is encountered less and less in the wild. Has that been your experience, too ? Recently ?
 
user666 said:
I heard that recently Meh is encountered less and less in the wild. Has that been your experience, too ? Recently ?
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I literally haven't found anything but meh, but I'm in the uk. I haven't bought anything since early this year but last time I looked online the descriptions seemed even worse than ever. Homogenous text about 'dutch fire' - the usual rubbish. All quite depressing.
 
Yeah, that seems to be the case. Although I suspect that those finding good stuff in those regions are from local connections rather than online?
 
Also, have you ever tried Fentanyl detection strips on the Meh ?
This makes sense because the same people that handle Fentanyl often handle other drugs, too (incl. MDMA) ...and because Fentanyl is so potent, the cross-contamination can happen inadvertently during handling (even more so with the more potent Fentanyl analogs).
I would do this myself but I do not have any Meh.

If the test is positive then I heard that removing Fentanyl (and analogs like Carfentanil and Lofentanil) contamination from MDMA can be done by exploiting their different pKA in AB extractions, because:
Fentanyl: 8.4pKa
Lo/Carfentanil: ~8.0pKa
MDMA: 9.9pKa
( a good pH meter is needed but the reagents are simple ).
 
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Since you gave me a thumbs up for the inadvertent Fentanyl cross-contamination, I'll reciprocate with a procedure to separate MDMA from Fentanyl and its analogs by exploiting their different pKA in AB extractions:
  • Dissolve: 1g sample of contaminated MDMA·HCl in 20mL warm distilled water.
  • Filter (e.g.coffee filter) → clear solution.
  • Basify: Slowly dilute with 1M solution of NaOH dropwise to pH 9.2-9.5 (use precise pH meter). Don't overshoot!
  • Extract: Add 50mL Xylene, shake 10min, wait for layers to separate (fentanyls go into the top organic layer - discard it).
  • Repeat: Repeat the former extraction 5x, maintain pH 9.2-9.5, discard all organic layers, keep the aqueous layers (do not reuse the same glassware).
  • Acidify: Dilute with HCl to pH 6 → MDMA·HCl crashes out.
  • Evap/Filter: Recrystallize from hot IPA/acetone (slowly cool → white crystals).

    Note: Toluene or Naphtha can be used in lieu of the Xylene.
I invite the more experienced chemists here to refine this procedure.
 
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ThreePointCircle said:
Very interesting. The frustration that has existed since the first page of the first thread is that analysis could answer the question, but the services available to the public tend to just say 'pure as the driven snow' while forensic papers always talk about contaminants relating to the synthesis procedures. I remember one of the authors of the MDDMA inhibitor paper was asked how much it would take to have the 'meh' effect, and while they didn't know, they speculated that it could be a small amount. So anything else in the sample could be relevant but goes unreported by the testing services.
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Did you ask for an inpurity report vs a what is this report?

A seperation with chromotrographyand analysis is the waay to go maybe with added HPLC that will you get the report you are looking for.

also maps grain size is .1 to .3 ckar
 
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