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Discriminating between saffrole and MDMA by reagents?

B

BigTrancer

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As the thread title suggests, I'm wondering about the possibility of reagent testers being able to discriminate between saffrole and MDMA. Some evidence is coming to light about speedbomb pills that have had saffrole added to them (pre-pressing I would assume), in order to fool a Marquis test. I can see why this would work, as both MDMA and saffrole should give a purple/black reaction to Marquis reagent.

What I'm curious about is to whether another reagent, or series of reagents could reliably and definitively discriminate between an MDMA-based pill, and any other combination of non-MDMA ingredients plus saffrole. Clearly, Marquis doesn't cut it for this application, but does anyone know the specifics on saffrole reacting with either Simon's, Mecke's or any other reagents?

BigTrancer :)
 
phase_dancer said:
Are all the drug users of the world simply too fucked to put together something of which the principles of operation are dead simple and have already been exploited for decades? Take into account the quality and price of VIS/UV detectors these days, and I reckon it wouldn't be impossible to build a computer operated unit which would sell for ~$1,000. If you think such a device would be instantly prohibited, think again. A simple change of column and solvent phases would make the unit applicable to the analysis of many substances ( and most amines use universal phases. What with the lack of proper labelling laws in Australia, and the recent example of quality control shown by PAN, such a device would undoubedly have a good market, even if its just to check that the food and pharmaceuticals you eat are up to standard.
Click to expand...

if you build it they will come... =D
 
BE CAREFUL with sass smelling pills. It should be more cause to test under ideal conditions, and if possible compare with a known MDMA tablet reaction.
 
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excellent work phase_dancer! at the vaada symposium where dr. cate quinn who is in charge of the police lab tests of seized pills spoke, she mentioned a statistic that in pills from 2002, 17% contained safrole. [im not exactly sure on that stat, but it was in that range]. i also dont know what amounts, or if it was simply unreacted during the synth but it is still enough to be aware of and take it into consideration when deciding on what pill to buy. it shows the limitations of reagent testers, but to limit the possibility of having an adulterated pill other sources should be used in conjunction such as as user reports from pillreports/friends.
 
Cowboy Mac, the figure of 17% is not that surprising, but as you indicate, it doesn't really tell us much either.

Safrole is often an impurity - up to ~1% - in commercially sourced MDP2P, and would probably be present even in carefully prepared *homemade* isosafrole and MDP2P. Other routes to MDMA such as wacker oxidation and bromosafrole methods would also leave unreacted safrole in the reaction product mixture.

But if the route involves the ketone and it is distilled, this should remove most if not all unreacted safrole, iso etc. Frequent washings following amination/ crystallisation should reduce this further again, certainly down to less than 1% content.

So of the 17% of tablets containing safrole, what needs to be asked is:
  • What amount of safrole was found in each tablet/batch tested?
  • What percentage of safrole containing tablets also contained MDMA or other drug?
  • Was the safrole distributed evenly through the tablet, or was it present only on the outer casing?

Answers to these questions would give a clearer picture as to whether this is a common practice, designed specifically to fool, or that it is more common for it to be the result of bad lab technique or unintended packaging/ pressing contamination.
 
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So how about Simon's? I would love to see a reaction of that and saffrole. And Mecke if you've got it.
 
So no change with Simon's? Interesting. Possibly a sequence of Marquis, Mandelin, Simon's, Robadope would show up such pills?
 
But BT's report indicated meth with safrole, in which case simons would give a positive.
 
Those interested might want to have a look at this from Microgram June 2003

Since the discovery by Dutt and Teo1 that spraying thin layer chromatographic (TLC) plates bearing drug spots
with ninhydrin produces a variety of colors that can distinguish between many drugs, this reagent has been
intensively used in this laboratory. The colors that are produced with ninhydrin, when correlated with the specific
migration values (Rf) for each spot on specific TLC plates and using select solvent systems, greatly enhance the
specificity of TLC for various drugs.
Click to expand...


I'm wondering if some of the analogues mentioned further along in the article could be used alone as colour indicators without employing TLC? Check out the chart on page 30, these 2 stuck out as being the most promising compounds, producing no background colour, but Reagent H lists similar colours for MDMA as for meth (purple / brown) Reagent F lists different colours for meth, amphetamine and MDMA/MDA, but who knows what a mixture of safrole and any of these would produce.

Reagent F ((3-oxo-2,3-dihydro-1H-inden-1-ylidene)malononitrile), at a working concentration of 2% w/v:
Intense brown-red spots are observed, mostly with amphetamines. In contrast, opiates (heroin, morphine) and
cocaine produce only low intensity red colored spots. No reaction is observed with LSD. At low drug
concentrations, the red colored background interferes with the colored spots.

Reagent H (4-chloro-7-nitro-2,1,3-benzoxadiazole), at working concentrations of 1.5 - 2% w/v: Intense brownpurple
spots are formed with amphetamines, yellow spots with narcotine and papaverine in opium, blue spots with
heroin, and brown spots with cocaine. An intense color reaction is also observed with LSD. In general, the colors
obtained are very similar to the colors developed with ninhydrin, but the sensitivity of H is higher; therefore, a
lower reagent concentration is required.
Click to expand...

This is probably a good place to start for someone looking for a more specific marker of MDMA, and possibly more specific indication of ring substitutions.

I know of two other proven reagents specific for methylene-dioxy groups, but on their own they would be of little value in distinguishing safrole & meth from MDMA
 
A well known test for alkenes is observing colour change from reaction with potassium permanganate. unfortunately this once everyday chemical is now restricted. But as luck would have it, for some unknown reason 2 years ago our field med cabinet stock up included a jar from Gilseal Home Care.

OK, getting back to the colour change. An acidified solution of KMnO4 is mixed with the suspect alkene and colour change is observed through the following reaction:

From The Chemistry of Organic Compounds (23)

alkenes with manganate(VII)
Acidified potassium managanate(VII) is decolourised by an alkene an a diol formed.
5CH2 = CH2 + 2H2O + 2MnO4- + 6H+ -----> 5HOCH2CH2OH + 2Mn2+ ethane -1,2 -diol
Click to expand...



EDIT

This is not an adequate test as described above. Edited 17-05-06
 
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Excellent demonstration - it certainly worked well.

Why on earth do they restrict permanganate - isnt it still available at pharmacies?

As a sidebar, the first reaction phase_dancer did was the exact colour reaction i have seen with sulphuric acid ONLY many moons ago when i was actually in a uni lab.

Its the sulphuric acid doing the work there - the presence of the other ingredients in marquis does not effect the colour change.

So i believe when MDXX amphetamines are tested the orange reaction "adds" together to make a far blacker/bluer colour change we are used to - not as violet as phase_dancer has shown.

This adds nothing to the question at hand but is a relevant, arguably useless, tidbit nonetheless.
 
Great work phase_dancer! You are not an arm-chair chemist after all :)

Biscuit: Potassium Permanganate is certainly OTC at pharmacies. It is a List III precursor because of its strong oxidation property which can be misused. How the two fit together beats me.
 
Hmmm... perhaps that is what they were referring to on the radio a couple of weeks ago when someone was saying how chemicals will be further restricted in WA when you'd think they couldn't restrict them any more. Next thing you know and distilled water will be on the List :)
 
Re: OTC everything


Ultimately, the wellbeing of the user is most threatened by the restriction of chemicals used in drug manufacture, as producers are required to involve more steps in the synthesis of a substance. The expected contaminants are far greater if all the precursors and reagents have to themselves be synthesised.

But alas, even in a country supposedly supporting harm reduction, I yet have no idea on how to convincingly present such an argument? - 8)

However, while drugs remain a health issue, I foresee eventual head on issues between Law and Health. I guess I see Health issues as being more a matter of scientific/ sociologic rationale, whereas Law is more of a moral implication based and built upon previous rulings. There are already more grey areas between these departments than ever before. I could be wrong but as I see it, sooner or later accountability and forced acknowledgement will be the basis for some serious policy changes worldwide.
 
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