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N-Methyl Hallucinogenic Amphetamine Analysis

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Chimitant:
Seems they investigated MDNA tablets contaminated with amphetamine and cocaine. Phtalates seem strange to me in a MDMA tablet, may be from plastic bags they have been stored in ?  What about compound 22? Is that used as a cutting agent?

pashov:
Hmm.. How does number 7 in "Impurity profiling of seized MDMA tablets by capillary gas chromatography" happen?

moo:
Probably by reductive amination of piperonal (no. 5) with methylamine.

methyl_ethyl:
Capillary Electrophoresis Analysis of a Wide Variety
of Seized Drugs
Ira S. Lurie Patrick A. Hays Kimberly Parker
Electrophoresis 2004, 25, 1580–1591
DOI:10.1002/elps.200405894


Capillary electrophoresis methodology is presented for the routine analysis of a wide variety of seized drugs using the same capillary with dynamic coatings and multiple run buffers. The types of exhibits analyzed using diode array UV detection include phenethylamines, cocaine, oxycodone, heroin, lysergic acid diethylamide (LSD), opium, hallucinogenic mushrooms, and G-Hydroxybutyrate G-butryolactone (GHB-GBL} Both qualitative and quantitative analyses are achieved using run buffers that contain additives that provide for secondary equilibrium and/or dynamic coating of the capillary. Dynamic coating of the capillary surface is accomplished by rapid flushes of 0.1 N sodium hydroxide, water, buffer containing polycation coating reagent, and a buffer containing a polyanionic coating reagent (with or without cyclodextrin(s)) or a micelle coating reagent. Dynamic coating with a polyanionic coating reagent is used for the analysis of moderately basic seized drugs and adulterants. The use of cyclodextrin in the run buffer not only allows for chiral analysis but also greatly enhances separation selectivity for achiral solutes. A capillary dynamically coated with a micelle allows for the analysis of neutral, acidic, and weakly basic drugs (GHB, GBL and neutral, acidic, and weakly basic adulterants). Dynamic coating, which gives rise to a relatively high and robust electroosmotic flow at pH, 7, allows for rapid, precise and reproducible separations. For a wide variety of drugs, excellent linearity and migration time precision and good peak area precision (external and internal standard) is obtained. Quantitative results for synthetic mixtures are in good agreement with actual values. Screening for adulterants is greatly enhanced by the use of automated library searches.

regards,

methyl_ethyl

Rhodium:
Analyses of impurities in methamphetamine by inductively coupled plasma mass spectrometry and ion chromatography
Shin-Ichi Suzuki, Hitoshi Tsuchihashi. Kunio Nakajima, Akira Matsushita, Takeo Nagao
J. Chrom. 437, 322-327 (1988) (https://www.thevespiary.org/rhodium/Rhodium/pdf/meth.impurity.analysis.icp-ms.pdf)
____ ___ __ _

Use of Bonded-Phase Silica Sorbents for Rapid Sampling of Impurities in Illicit Amphetamine for High-Performance Liquid Chromatographic Analyses
Marit Lambrechts and Knut E. Rasmussen
J. Chrom. 331, 339-348 (1985) (https://www.thevespiary.org/rhodium/Rhodium/pdf/amph.impurity.sampling.pdf)

Summary
A simple and rapid method has been developed for the extraction of impurities from illicit amphetamine samples using bonded-phase silica sorbents. The drug is dissolved in phosphate buffer (pH 7) and added to a C8 Bond Elut™ extraction column. The column is washed with water, and the impurities are then eluted with acetonitrile. The eluate is directly injected into the liquid chromatograph. This sample preparation technique has been compared with the traditional liquid–liquid extraction method. High-performance liquid chromatographic analysis of the impurities is carried out on a reversed-phase C18 column with an acetonitrile–water gradient as mobile phase. Peaks are monitored by UV detection at 220 and 254 nm. A series of seized amphetamine samples has been analysed, and the procedure gives detailed impurity patterns suitable for the comparison of samples. Compounds are identified by absorbance ratios (A220/A254).

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