Helmut Neumann

Heroin impurity profiling : A harmonization study for retrospective comparisons

Three laboratories present a harmonised system for the retrospective comparison of south west Asian heroin. It consists of an improved gas chromatographic (GC) profiling method and a computerised data retrieval. The investigations of the GC were necessary with a view to improve the reproducibility of the system. The necessity of a strict quality control is emphasized. The peaks of the GC profile were investigated for abundance, intensity, GC behaviour (reproducibility) and correlations; 16 of them were selected for describing the heroin profile in the database. The results from intra-lab profile comparisons are reported. The reproducibility of the analysis was good and the variation between the samples was large, thus, allowing conclusions with a high degree of certainty. The criteria of similarity were defined. The system is successfully running in all three labs. In connection with inter-laboratory comparison, the aspects of method harmonisation and standardisation are discussed. It appeared that the GC method is a very subtile one, urging for a strict standardisation between the three labs. Despite a long cooperation between three well-equipped and experienced labs, a more or less serious loss of reproducibility was noticed in the inter-lab results in comparison with the intra-lab results. The loss could for the greater part be attributed to the (limits of the) GC technique; a number of compounds, necessary for making the discrimination between samples, showed difficult chromatographic behaviour, leading to insufficient inter-lab reproducibility. Using the actual variables, improvements in performance can hardly be expected in the near future. The loss of reproducibilty implies that the number of false positive matches in a database search increases. This may strongly reduce the value of a relatively large, international database. The study shows that so far, the best option for international comparison is the analysis in a central laboratory. The idea of local determination at a large number of national labs and the use of a common database is not a realistic aim for this type of analysis.

Comparison of heroin by capillary gas chromatography in Germany

The situation in Germany over the last 12 years concerning illicit heroin seizures and forensic analytical research devoted to the comprehensive characterization of this dangerous drug has been reviewed. Major developments include the harmonization of chromatographic analytical methods for quantitation of heroin and the major alkaloids and derivatives within the network of state and federal forensic science laboratories, classification of illicit heroin according to known processing patterns, impurity profiling of organic trace components using capillary gas chromatographic analysis and robotics for automated sample preparation, and the comparison and evaluation of the generated complex analytical data by advanced computerized methods.

Determination of δ13 CV−PDB and δ15NAIR values of cocaine from a big seizure in Germany by stable isotope ratio mass spectrometry†

In this study, δ13CV− PDB and δ15NAIR values of 132 cocaine samples from a big seizure in Germany in 2002 were determined using elemental analyser isotope ratio mass spectrometry. The 1.2 tons of cocaine were packed in 1 kg packages and the cocaine bricks inside these packages showed certain logos. Twenty different logos could be identified. Results show a large variability among some samples, for δ15NAIR values ranging from−17 to −2 ‰. Furthermore, the possibility of linking samples with the same logo was checked. The results show that, in general, there is no relationship between the determined isotope ratio and a certain logo. †Extended version of a paper presented at the 26th Annual Meeting of the German Association for Stable Isotope Research (GASIR), 10–12, October, 2005, Jena, Germany.

Nachweis von 3-O-Acetylmorphin als Zersetzungsprodukt des Diacetylmorphins (Heroin) mit HPLC und Capillar-GC

SummaryThe decomposition of diacetylmorphine under various conditions (pH-value, temperature) was studied. The decomposition products were quantified by means of HPLC and capillary GC. 3-O-Acetylmorphine was identified in all decomposition tests besides 6-O-acetylmorphine and morphine. Ratios of the concentrations of the two acetylmorphine isomers were determined for illicit heroin samples. The application of the ratios for characterizing heroin samples is discussed.ZusammenfassungEs wurde die Zersetzung von Diacetylmorphin unter verschiedenen Bedingungen (pH-Wert, Temperatur) untersucht. Die Quantifizierung der Zersetzungsprodukte erfolgte mit HPLC und Capillar-GC. Bei allen Zersetzungsversuchen konnte die Bildung von 3-O-Acetylmorphin neben 6-O-Acetylmorphin und Morphin nachgewiesen werden.Für illegale Heroinproben wurden Verhältniszahlen aus den Konzentrationen der beiden Isomere bestimmt. Ihre Verwendung zur Charakterisierung von Heroinproben wird diskutiert.