Characterization of a heroin manufacturing process based on acidic extracts by combining complementary information from two-dimensional gas chromatography and high resolution mass spectrometry

- A comprehensive two-dimensional gas chromatography mass spectrometric approach (GC×GC-TOFMS) supported by one-dimensional gas chromatography high resolution mass spectrometers (GC-HRTOFMS, GC-FTICRMS) were used to track and confirm characteristic chemical impurities through an authentic illicit heroin production process.

A comprehensive two-dimensional gas chromatography mass spectrometric approach (GC×GC-TOFMS) supported by one-dimensional gas chromatography high resolution mass spectrometers (GC-HRTOFMS, GC-FTICRMS) were used to track and confirm characteristic chemical impurities through an authentic illicit heroin production process. Minor and trace compounds present in illicit heroin that result from the used opium and the manufacturing process generate a specific impurity profile of each batch. Based on that, comparative analysis of heroin samples is possible, which can contribute amongst others to the uncovering of links between seized samples. The illicit manufacturing processes are thereby only vaguely described in the literature. Neutral and acidic compounds of the unadulterated impurity profiles at different stages during an authentic manufacturing process of heroin were analyzed by comprehensive two-dimensional gas chromatography - time-of-flight mass spectrometry (GC×GC-TOFMS). The focus was set on 44 compounds, mostly acetylation products, found in the heroin base including four unaltered opium alkaloids and 18 target compounds used within the German Heroin Analysis Program (HAP) at the Bundeskriminalamt (Federal Criminal Police Office; BKA). 12 compounds were found to be preserved unaltered through the manufacturing process. In case of 21 acetylated compounds the original alkaloid is known or could be assigned, i.a. by analysis of separately acetylated standards.Using GC coupled to high resolution time-of-flight mass spectrometry (GC-HRTOFMS), major fragments caused by electron impact ionization (EI) were determined. The corresponding molecular weight was obtained by GC hyphenated to Fourier transform mass spectrometry mass spectrometer (FTICRMS) via atmospheric pressure chemical ionization (APCI) as soft ionization interface.

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