Development of a harmonised method for the profiling of amphetamines V: Determination of the variability of the optimised method

This paper is the fifth in a series of six in relation to the development of a harmonised method for the profiling of amphetamine [L. Aalberg, K. Andersson, C. Bertler, H. Borén, M.D. Cole, J. Dahlén, Y. Finnon, H. Huizer, K. Jalava, E. Kaa, E. Lock, A. Lopes, A. Poortman-van der Meer, E. Sippola, Development of a harmonised method for the profiling of amphetamines I. Synthesis of standards and compilation of analytical data, Forensic Sci. Int. 149 (2005) 219-229; L. Aalberg, K. Andersson, C. Bertler, M.D. Cole, Y. Finnon, H. Huizer, K. Jalava, E. Kaa, E. Lock, A. Lopes, A. Poortman-van der Meer, E. Sippola, J. Dahlén, Development of a harmonised method for the profiling of amphetamines II. Stability of impurities in organic solvents, Forensic Sci. Int. 149 (2005) 231-241]. The third paper [K. Andersson, K. Jalava, E. Lock, L. Aalberg, Y. Finnon, H. Huizer, E. Kaa, A. Lopes, A. Poortman-van der Meer, M.D. Cole, J. Dahlén, E. Sippola, Development of a harmonised method for the profiling of amphetamines III. Development of the gas chromatographic method, Forensic Sci. Int., in press] dealt with the optimisation of the gas chromatographic and detection methods whereas the fourth paper [K. Andersson, K. Jalava, E. Lock, Y. Finnon, S. Stevenson, L. Aalberg, H. Huizer, E. Kaa, A. Lopes, A. Poortman-van der Meer, M.D. Cole, J. Dahlén, E. Sippola, Development of a harmonised method for the profiling of amphetamines IV. Optimisation of sample preparation, Forensic Sci. Int., in press] concerned the optimisation of the extraction method prior to GC analysis. This paper is a study of the optimised method in order to determine its stability. Investigations of within and between day variations were carried out in four laboratories. Moreover, variations between laboratories were also determined. Both flame ionisation detector (FID) and MS detection were used. One laboratory studied nitrogen-phosphorous detector (NPD) detection as well. For this task, 12 batches of amphetamine were prepared. Six of them were synthesised via the Leuckart route, three via the nitrostyrene route and three via the reductive amination route [A.M.A. Verweij, Impurities in illicit drug preparations: amphetamine and methamphetamine, Forensic Sci. Rev. 1 (1989) 2-11]. Taking into account all studied target compounds and the average results from four laboratories, the within day variation was around 6% for FID and 5% for MS, the between days variation was around 10% for FID and 8% for MS. For NPD detection, within day variation was 5% and between days variation 9% (only one laboratory). Finally, the inter-laboratory variation was about 12% for FID (four laboratories) and 10% for MS (three laboratories).     

Analytical profile of 4-methylthioamphetamine (4-MTA), a new street drug

The analytical properties for a new street drug, 4-methylthioamphetamine (4-MTA), are presented. This new compound was found in tablets sold on the illicit market in the Netherlands and Switzerland in 1997 and 1998. The intermediate 1-(4-methylthiophenyl)–2-nitropropene was also found in a clandestine laboratory in the Netherlands in January 1997.In this study, reference standards were prepared and characterized. The ultraviolet, infrared and nuclear magnetic resonance spectral properties as well as the chromatographic and mass spectrometric (MS) data are reported.     

Development of a harmonised method for the profiling of amphetamines: IV. Optimisation of sample preparation

The suitability of liquid-liquid extraction (LLE) and solid-phase extraction (SPE) for the preparation of impurity extracts intended for gas chromatographic profiling analyses of amphetamine were evaluated. Both techniques were optimised with respect to the extraction of selected target compounds by use of full factorial designs in which the variables affecting the performance were evaluated. Test samples consisted of amphetamine synthesised by the Leuckart reaction, by reductive amination of benzyl methyl ketone and by the nitrostyrene route. The performance of LLE and SPE were comparable in terms of repeatability and recovery of the target compounds. LLE was considered the better choice for the present harmonised amphetamine profiling method due to the lack of information on the long-term stability of SPE columns.     

Access to health care for undocumented migrants: a comparative policy analysis of England and the Netherlands

The presence of undocumented migrants is increasing in many Western countries despite wide-ranging attempts by governments to increase border security. Measures taken to control the influx of immigrants include policies that restrict access to publicly funded health care for undocumented migrants. These restrictions to health care access are controversial, and evidence suggests they do not always have the intended effect. This study provides a comparative analysis of institutional, actor-related, and contextual factors that have influenced health care policy development on undocumented migrants in England and the Netherlands. For undocumented migrants, England restricts its access to care at the point of service, while the Netherlands restricts through the payment system for services. The study includes an analysis of policy papers and semistructured, in-depth interviews with various actors in both countries. Findings confirm the influence of such contextual factors as immigration considerations and cost concerns on health care policy making in this area. However, these factors cannot explain the differences between the two countries. Previously enacted policies, especially the organization of the health care system, affected the kind of restrictions for undocumented migrants. Concerns about the side effects of generous treatment of undocumented migrants on other groups played a substantial role in formulating restrictive policies in both countries. Evidently, policy development and implementation is critically affected by institutional rules, which govern the degree of influence that doctors and professional medical associations have on the policy process.     

Development of a harmonised method for the profiling of amphetamines: III. Development of the gas chromatographic method

This study focused on gas chromatographic analysis of target compounds found in illicit amphetamine synthesised by the Leuckart reaction, reductive amination of benzyl methyl ketone, and the nitrostyrene route. The analytical method was investigated and optimised with respect to introduction of amphetamine samples into the gas chromatograph and separation and detection of the target substances. Sample introduction using split and splitless injection was tested at different injector temperatures, and their ability to transfer the target compounds to the GC column was evaluated using cold on column injection as a reference. Taking the results from both techniques into consideration a temperature of 250 degrees C was considered to be the best compromise. The most efficient separation was achieved with a DB-35MS capillary column (35% diphenyl 65% dimethyl silicone; 30 m x 0.25 mm, d(f) 0.25 microm) and an oven temperature program that started at 90 degrees C (1 min) and was increased by 8 degrees C/min to 300 degrees C (10 min). Reproducibility, repeatability, linearity, and limits of determination for the flame ionisation detector (FID), nitrogen phosphorous detector (NPD), and mass spectrometry (MS) in scan mode and selected ion monitoring (SIM) mode were evaluated. In addition, selectivity was studied applying FID and MS in both scan and SIM mode. It was found that reproducibility, repeatability, and limits of determination were similar for FID, NPD, and MS in scan mode. Moreover, the linearity was better when applying FID or NPD whereas the selectivity was better when utilising the MS. Finally, the introduction of target compounds to the GC column when applying injection volumes of 0.2 microl, 1 microl, 2 microl, and 4 microl with splitless injection respectively 1 microl with split injection (split ratio, 1:40) were compared. It was demonstrated that splitless injections of 1 microl, 2 microl, and 4 microl could be employed in the developed method, while split injection and splitless injections of 0.2 microl should be avoided.     

Corruption prevention: A course for police officers fighting organised crime

In literature one often finds education and training are given as possible prevention methods to cope with corruption but with little evidence or information on how to deal with the problem of how to set up such a course. This article is about the course set up by the College for Criminal Investigation and Crime Control, the Netherlands, concerning corruption prevention training for police officers. The aim of this course is for participants to gain insight into their own decision process; that they decide, what they decide and what the consequences of their decisions can be. Gaining insight is intended to make them less vulnerable to corruption. It is a three-day course in which corruption prevention is approached from an individual point of view. The article will start with a theoretical framework,after which the course is described. It offers a practical means of addressing an issue that attracts much attention but little guidance on its resolution. This revised version was published online in July 2006 with corrections to the Cover Date.     

Development of a harmonized method for the profiling of amphetamines. I. Synthesis of standards and compilation of analytical data

Reference material was synthesised for 21 substances that are frequently present as synthetic impurities, i.e. by-products, in illicitly produced amphetamine. Each of these substances is a typical by-product for at least one of the three approaches most often used to synthesise amphetamine, namely, the Leuckart, the reductive amination of benzyl methyl ketone, and the nitrostyrene routes. A large body of data on the substances was recorded, including the following: mass spectra, ultraviolet spectra, Fourier transform infrared spectra, infrared spectra in gas phase, and 1H NMR and 13C NMR spectra.     

Development of a harmonized method for the profiling of amphetamines. II. Stability of impurities in organic solvents

The present study focused on the stability of 22 amphetamine impurities dissolved in six organic solvents: isooctane, toluene, ethanol, dichloromethane, ethyl acetate, and diethyl ether. The aim was to find the most inert, and thereby most suitable, solvent for amphetamine profiling. Mixtures of the impurities were prepared in the different solvents, and changes in the concentrations of the individual compounds over-time were monitored by gas chromatographic analysis after 0, 4, 12, 24, 48, and 96 h. Isooctane and toluene provided the most inert conditions, although, a few of the impurities were insufficiently stable in these two solvents. The present experiments were performed as a part of the development of a harmonized method for profiling of amphetamine. The results can be used to support the choice of organic solvents for sample preparation. They also provide information about the stability of the impurities that are found in profiles of illicit amphetamine. This is essential due to the fact, that unstable compounds can have a negative influence on the comparison of profiles.     

Trends in the Reaction on Crime in Criminal Justice Systems in Europe in 1990–2007: A Comparison of Four European Regions

Recorded crime and prison populations seem to be increasing in Europe. Some explanations for this situation can be related to changes in the reaction on crime by the Criminal Justice Systems. The information collected in the European Sourcebook of Crime and Criminal Justice Statistics (ESB) provides a good opportunity to look in more detail at the changes in the various stages of the Criminal Justice Systems in more than 40 European countries over the period 1990 to 2007. In this study we look mainly at the changes over time of recorded crimes, the offender ratio, the conviction ratio and punitivity in Europe where the countries are clustered into four regions: North/West, South, Central and East Europe. It was found that the increase in the number of recorded drug crimes and a possible higher priority for violent crimes could help explain the increase in recorded crimes during the last two decades. The Criminal Justice Systems in Europe, with some differences between regions within Europe and despite not having more police resources, succeed in finding more offenders. The conviction ratio appeared to be increasing as well, mainly in Central Europe. While punitivity for Europe as a whole is stable, there are vast differences in the levels and trends between the regions.     

Development of a harmonised method for the profiling of amphetamines VI: Evaluation of methods for comparison of amphetamine

Amphetamine samples were analysed by gas chromatography-mass spectrometry (GC-MS), and the peak areas of 33 target compounds were transformed by applying various pretreatment techniques. The objective was to optimise the ability of a number of distance metrics to establish links between samples of amphetamine originating from the same batch (henceforth referred to as linked distances). Furthermore, partial least squares discriminant analysis (PLS-DA) was used to evaluate the effects of various pretreatment methods on separation of amphetamine batches synthesised by the Leuckart reaction, reductive amination of benzyl methyl ketone, and the nitrostyrene route. The most efficient way to pretreat GC-MS data varied for the different distance metrics, although best results were obtained when data were normalised to the sum of peak areas, and either the fourth root or a logarithm was applied to the normalised data. When pretreating normalised data by fourth root transformation, Pearson correlation was the distance metric that was most successful at finding linked samples. Normalisation and the use of fourth root also represented the best method of pretreating data when employing PLS-DA to separate samples synthesised by different routes. To achieve a faster and more user-friendly procedure for evaluating chromatograms, experiments were performed in which the number of target compounds used to compare samples was reduced. The effect of each compound that was removed was studied by applying PLS-DA and by using Pearson correlation to calculate linked distances as well as unlinked distances (between samples from different batches of amphetamine). Considering both links between samples from the same batch and separation of samples synthesised by different routes, the best results were obtained with the data set comprising 26 compounds. Finally, it was found that the profiling method developed in this work was superior to an existing technique with respect to separating linked and unlinked distances.