Materialvergleichsuntersuchungen ausgewählter Rauschgifte mittels Kapillarelektrophorese-Elektrospray-Ionisations- und mittels Gaschromatographie-Elektronenstoß-Ionisations-Massenspektrometrie

3,4-Methylenedioxymethamphetamine-hydrochloride (MDMA-HCl) is typically the main active substance in Ecstasy tablets. In this work the influence of different reaction conditions (temperature, reaction time, pressure and chemical origin of precursor batch) on the organic impurity profiles of MDMA resulting from the reductive amination via PtO2/H2 was examined. The variation of the reaction temperature as well as the change of precursor batch has a large impact on the resulting impurity profile. By using the target compounds of the internationally applied harmonised profiling GC-MS method, an accurate classification of all samples derived from the same synthetic route (same reducing agent) was prevented due to the impact of the variation of reaction temperature or change of the precursor batch on the impurity profile. This can lead to misinterpretation of the profiling results. Variation of the conditions during the precipitation step has also influence on the organic impurity profiles of the end product, but less than the influence due to a change of the reducing agent. The profiling result strongly depends on the selected target compounds. Most of the illicit drugs and some adulterants occur as optical isomers with different psychotropic activities. Especially for illicit methamphetamine and Ephedra alkaloid samples not only the enantioselective determination of the active substance but also the enantioselective determination of the chiral impurities is important for intelligence purposes with respect to the discrimination of different production batches. Therefore it is important to have a flexible and sensitive analytical method for the chiral separation and unambiguous identification of drugs and adulterants belonging to different families of compounds. In this work a CE-ESI-MS method was optimized which allows the chiral identification of different drugs, adulterants and impurities. Enantiomeric resolution was achieved by adding cyclodextrins to the running buffer. With the developed method it was also possible to discriminate between different batches of illicit methamphetamine samples by comparing their chiral impurities. The chiral CE-DAD method, which was described in this work, is also suitable for the discrimination between different batches of methamphetamine samples by comparing their chiral impurities, but this method has less sensitivity and an unambiguous identification of the trace components is not possible. The identification power and sensitivity of the chiral analysis was increased by using CE-ESI-MS. In addition, an achiral CE-ESI-MS procedure was optimized for the chemical profiling of heroin and cocaine samples. Because of its high matrix tolerance, CE is often used for the chemical profiling of heroin and cocaine. To obtain higher sensitivity and selectivity, capillary electrophoresis coupled to mass spectrometry was applied in this work. The additives and by-products in several seized heroin and cocaine samples were analysed and quantified using this CE-ESI-MS-method. It was possible to discriminate between different batches of cocaine samples and different batches of heroin samples by comparing the additives and by-products. In comparison to the GC-MS methods routinely used for the chemical profiling of heroin and cocaine, no time consuming sample preparation is required when using the CE-ESI-MS method. The results of this work show the suitability of capillary electrophoresis coupled with mass spectrometry as an analysis method for the organic profiling of a wide range of drugs of abuse. It was possible to discriminate between different batches of illicit drug samples by comparing the main active substance as well as the by-products, additives and impurities. The analysis method is also suitable for the chiral identification of a wide range of drugs and adulterants.