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N-Methyl Hallucinogenic Amphetamine Analysis

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Rhodium:
Hydrastinin: An Impurity in 3,4-(Methylenedioxy)methamphetamine
Anthonie M. A. Verweij
Arch. Krim. 188(1-2), 54-57 (1991) (https://www.thevespiary.org/rhodium/Rhodium/pdf/forensic/mdma.hydrastinin.pdf)
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Impurities in illicit amphetamine 6.
Identification of phenyl-2-propanol, amphetamine and N,N-dimethylamphetamine in methamphetamine
A. M. v. d. Ark, A. B. E. Theeuwen and A. M. A. Verweij
Arch. Krim. 162, 171-175 (1978) (https://www.thevespiary.org/rhodium/Rhodium/chemistry/amph.impurities-6.html)

Summary
By means of GC-MS analysis three impurities, amphetamine, N,N-dimethylamphetamine and phenyl-2-propanol could be found in methylamphetamine synthesized by a high pressure reductive amination of methylamine and benzylmethylketone.

methyl_ethyl:
Analysis of illicit amphetamine seizures by capillary zone
electrophoresis
Veronique Piette, Frans Parmentier
Journal of Chromatography A, 979 (2002) 345–352



Abstract:

Capillary zone electrophoresis was applied for the determination of amphetamine and related substances in seized drugs. A
buffer made of 0.1 M phosphoric acid adjusted to pH 3.0 with triethanolamine was selected. With this background
electrolyte, triethanolamine is adsorbed to the capillary wall and the electroosmotic flow is reversed. This gives rise to peaks
with good symmetry, high efficiency and reproducible migration times. The separation of the different analytes was
performed in a fused-silica capillary thermostatted at 25 8C and the applied voltage was 25 kV. Under these experimental
conditions, amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine
(MDMA), 3,4-methylenedioxyethamphetamine, N-methyl-1-(1,3-benzodioxol-5-yl)-2-butamine and ephedrine were resolved
within 8 min and without interference from adulterants usually found in illicit powders. Their identification by the migration
time was confirmed by their UV spectra recorded with a diode array UV detector (190–350 nm). The selected method was
then applied to identify these substances in illicit tablets known as ‘‘Ecstasy’’ and the MDMA determined in these samples
according to a laboratory validation procedure.

Rhodium:
N-Ethyl-2-(3,4-methylenedioxyphenyl)-propan-1-amin eine neue Designerdroge mit der Struktur eines beta-isomeren MDE
P. Rösner, L. Zechlin, Th. Junge
Toxichem + Krimtech 70(2), 82-86 (2003) (https://www.thevespiary.org/rhodium/Rhodium/pdf/forensic/n-ethyl-2-%5B3.4-methylendioxyphenyl%5D-1-propanamin.beta-mde.pdf)
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[New, previously unavailable on the illegal drug market amphetamine derivatives with a partial propiophenone structure]
Fritschi G, Klein B, Rösner P
Arch Kriminol. 200(1-2), 8-16 (1997) (https://www.thevespiary.org/rhodium/Rhodium/pdf/34-md-2-pyr-propiophenone.pdf)

Abstract
Two new clandestine synthesized derivatives of amphetamine were seized in the FRG. They show a propiophenone-structure. A well known representative of this class of compounds is 2-Diethylaminopropiohenone. The compounds are not submissed under the German law. NMR, IR- and MS-datas of these compounds and additionally synthesized derivatives are reported.

Rhodium:
Contamination of Clandestinely Prepared Drugs with Synthetic By-products
William H. Soine
NIDA Monograph #95, pp. 44-50 (1989) (https://www.thevespiary.org/rhodium/Rhodium/chemistry/amphetamine-cocaine.impurities.html)

Rhodium:
Impurity profiling of methamphetamine hydrochloride drugs seized in the Philippines
Fabian M. Dayrit and Morphy C. Dumlao
Forensic Science International 144(1), 29-36 (2004) (https://www.thevespiary.org/rhodium/Rhodium/pdf/forensic/meth.hcl.impurities.philippines.pdf)

Abstract
Methamphetamine hydrochloride is one of the most widely used illicit drugs in the Philippines. In this study, we describe the application of cluster analysis of trace impurities in the profiling of the seized methamphetamine drug samples.
Thirty milligrams of a homogenized drug sample were dissolved in 1 mL of pH 10.5 buffer solution and extracted with ethyl acetate containing three internal standards. The trace impurities were identified using gas chromatography–mass spectrometry (GC–MS) and quantified by gas chromatography with a flame ionization detector (GC–FID).
Following previously reported methodologies, 30 impurity peaks were selected from the GC–FID chromatograms. The peak areas and retention times were referenced to the internal standards. The peak areas of the selected peaks were then grouped for cluster analysis. In order to check for consistency of clustering, two further cluster analyses were performed using 40 and 50 impurity peaks. Changes in clustering were observed in going from 30 to 40 impurity peaks, while analyses using 40 and 50 impurity peaks gave similar results. Thus, for the seized drug samples used in this study, cluster analysis using at least 40 impurity peaks showed better consistency of clustering as compared to analysis using 30 peaks only.
Ten of the impurity peaks were identified, of which four were identified for the first time in methamphetamine drug samples. These are p-bromotoluene, N-benzyl amphetamine, N-ethyl amphetamine, and N-ethyl methamphetamine. The presence of phenyl-2-propanone (P2P), N,N-dimethyl amphetamine, and N-formyl amphetamine is indicative that these casework samples were synthesized using the Leuckart method.
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Profiling of impurities in illicit methamphetamine by HPLC and capillary electrochromatography
Ira S. Lurie, Christopher G. Bailey, Deon S. Anex, M. Jason Bethea, Timothy D. McKibben, John F. Casale
Journal of Chromatography A, 870, 53–68 (2000) (https://www.thevespiary.org/rhodium/Rhodium/pdf/meth.impurity.profiling.pdf)

Abstract
High performance liquid chromatography (HPLC) with photodiode array (PDA) UV and fluorescence (FL) detection, and capillary electrochromatography (CEC) with laser-induced fluorescence (LIF) detection were investigated for the analysis of acidic extracts derived from illicit methamphetamine. These compounds include major impurities from the hydriodic acid/red phosphorous reduction method, i.e., 1,3-dimethyl-2-phenylnaphthalene and 1-benzyl-3-methylnaphthalene, and other trace-level, structurally related impurities. For certain of these solutes, HPLC with conventional FL detection gave at least a 603 increase in sensitivity over UV detection. In addition, other highly fluorescent impurities were detected in methamphetamine produced via four other synthetic routes. The use of a rapid scanning FL detector (with acquisition of ‘‘on the fly’’ excitation or emission) provided structural information and gave ‘‘optimum’’ excitation and emission detection wavelengths. CEC with LIF detection using UV laser excitation provided greatly improved chromatography over HPLC, with good detection limits in the low ng/ml range. Both methodologies provide good run-to-run repeatability, and have the capability to distinguish between samples.

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