Abstract:
The illicit production of the synthetic drug amphetamine is expanding worldwide, especially in Europe. Amphetamine is predominantly synthesized via the Leuckart route in clandestine laboratories, which is characterized by its feasibility. However, this route comes along with a large amount of emerging production waste. Synthetic drug production confronts authorities with several challenges concerning an alternating designer pre-precursor market, detection of clandestine laboratories, their assessment after dismantling and finally environmental crimes that are related to the production process. The latter includes the illegal disposal of production waste in the environment. Open questions are, for instance, if chemical analyses can help to establish links between samples associated with disposal (production waste, contaminated environmental samples) and clandestine laboratories or if the extent of environmental pollution can be assessed. This thesis focuses on the characterization of production waste samples from amphetamine synthesis via the Leuckart route from dismantled laboratories and from dumpsites discovered in recent years and detection possibilities of production waste disposal in the environment.
In the case of dismantling a large-scale amphetamine laboratory or detection of a dumpsite with production waste, a large number of samples is seized. Their analysis necessitates fast analytical techniques. In this thesis, an ambient ionization – high-resolution mass spectrometry approach was tested for the rapid assessment of samples. The investigated approach neither required sample preparation nor chromatographic separation but allowed to identify synthesis markers and to discriminate samples by multivariate data analysis after direct injection for mass spectrometric analysis. Moreover, a classification model was developed, allowing discrimination of the four main types of amphetamine production waste from the Leuckart route.
In-depth characterization of samples from dismantled large-scale laboratories is required to understand production characteristics. Analysis of seized samples from a large-scale laboratory, in which producers applied the designer pre-precursor methyl α-phenylacetoacetate to obtain the key reaction educt benzyl methyl ketone and a modified version of the second synthesis step of the established Leuckart route, was accomplished by a nontargeted liquid chromatography – high-resolution mass spectrometry approach. This methodology identified synthesis markers for the Leuckart route and indicated the presence of novel synthesis markers for changes in the production process.
Some of these markers were further investigated with regard to illegal waste disposal. Deliberately disposing production waste at dumpsites is a cause for environmental concern and data on the fate of production waste in soil environment is scarce. The stabilities of five amphetamine synthesis markers, characteristic for the Leuckart route and identified in production waste, were investigated in soil using gas chromatography – and liquid chromatography – mass spectrometry. Four of these key compounds showed sufficient stability for at least four weeks. Amphetamine was identified as a biotransformation product of one compound in soil. The analysis of soil cores from a real case dumpsite revealed that there is a risk of synthesis markers leaching into deeper soil layers. The results demonstrated the potential for authorities to identify environmental crimes and to deduce the nature of the disposed waste at dumpsites and the environmental risks related to it.
Another way of disposing production waste is via the local sewer networks. New analytical tools were developed to identify synthesis markers in wastwater, ideally helping authorities to identify clandestine laboratories. A procedure to extract synthesis markers from wastewater samples with user-friendly polydimethylsiloxane rods in combination with gas chromatography – mass spectrometry methods was developed, which could even be performed on-site with transportable instruments. Additionally, a mobile sampling unit was successfully applied in the sewer for time-resolved detection of controlled production waste discharges, which indicated to be a valuable tool for potential monitorig of production waste discharges and localization of clandestine laboratories via the sewer system.
In summary, this thesis provides innovative and comprehensive methods for the assessment of the production waste in clandestine amphetamine laboratories. The results underline the associated environmental risks of synthetic drug production and facilitate criminal prosecution.
amphetamine-type stimulants