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N-Methyl Hallucinogenic Amphetamine Analysis

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Natrix:
Identificazione della 4-bromo-2,5-dimetossiamfetamina (DOB) in compresse clandestine sequestrate in Italia
FURNARI, OTTAVIANO, ROSATI
Ann. Ist. Super. Sanità, vol. 37, n. 2 (2001), pp. 297-300 (http://www.iss.it/publ/anna/2001/2/372297.pdf)

Summary
(Identification of the 4-bromo-2,5-dimetoxyamphetamine (DOB) encountered in illicit tablets seized in Italy)
Some of the molecules belonging to the amphetamines group (4-bromo-2,5-dimethoxyamphetamine, DOB) or to the phenethylamines (4-bromo-2,5-dimethoxy-phenethylamine, 2C-B or Nexus) have closely related structures that make their identification quite difficult. The unambiguous identification is crucial in forensic responses. This paper describes the analytical approach used to achieve the identification of the main ingredient contained in tablets seized in the illicit market of Rome (Italy) and submitted to our laboratory by the Court of Law of Rome. The procedure entails the basic extraction of the main ingredient from the tablets with tert-butyl methyl ether followed by qualitative gas chromatographic mass-spectrometric (GC-MS) analysis using both electron impact detection (EI) and chemical ionization (CI). The examination of the mass spectra obtained from the native molecule and from its pentafluoropropionyl-derivative allows the structural identification of the side chain and the substitutions on the aromatic ring. This analytical approach can thus be useful to distinguish between amphetamine-like and phenetylamine-like compounds using instruments and techniques commonly available in the forensic toxicology laboratories.

methyl_ethyl:
I swore I posted this previously however it is not coming up in the search engine.

Determination of MDMA, MDEA and MDA in urine by high
performance liquid chromatography with fluorescence detection
Jos Luiz da Costa, Alice Aparecida da Matta Chasin
Journal of Chromatography B, 811 (2004) 41–45
DOI:10.1016/j.chromb.2004.03.076


Abstract:
This paper describes the development and validation of analytical methodology for the determination of the use of MDMA, MDEA and
MDA in urine. After a simple liquid extraction, the analyses were carried out on a high performance liquid chromatography (HPLC) in an
octadecyl column, with fluorescence detection. The mobile phase using a sodium dodecyl sulfate ion-pairing reagent allows good separation
and efficiency. The method showed good linearity and precision. Recovery was between 85 and 102% and detection limits were 10, 15 and
20 ng/ml for MDA, MDMA and MDEA, respectively. No interfering substances were detected with fluorescence detection.


Question for all y'all chromatographic professionals.

I notice that the y axis in the chromatograms in the above pdf. is measured in %f.  I have found this is the norm when dealing with hp 1049 detectors usually running chemstation software.  I am not a fan of chemstation software, nor do I favor Agilent/HP Liquid Chromatographs.  I have found that Waters LC's running Empower/Milennium and using a Waters 474 fluorescence detector measure mV along the Y axis, which makes sense to me.  I was wondering if anyone actually knows what %f is.  I would assume that it could not simply be % of total fluorescence (because it does not add up that way).  My problem lies in transferring a method from an Agilent platform running chemstation to a Waters platform running Empower Software.  Perhaps the actual difference lies in how the detectors actually measure the fluorescence.  If this is the case I doubt there would be an accurate means of comparing the two detectors/Platforms.

Any thoughts/comments on the topic would be greatly appreciated.

much_love

methyl_ethyl

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