Determination of Neutral Manufacturing Impurities in Heroin by Capillary Gas Chromatography with Electron Capture Detection after Reduction with Lithium Aluminum Hydride and Derivatization with Heptafluorobutyric Anhydride

Article abstract of DOI:10.1021/ac00297a005

Neutral byproducts associated with the manufacture of illicit heroin are many and include meconin, 4-acetoxy-3,6-dimethoxyphenanthrene, N,O⁶-diacetylnorcodeine, 4-acetoxy-3,6-dimethoxy-5-<2-(N-methylacetamido)ethyl>phenanthrene, N,O³,O⁶-triacetylnormorphine, and 4-acetoxy-3,6-dimethoxy-8-<2-(N-metnylacetamido)ethyl>phenanthrene.These N- and O-acetylated impurities, and meconin, are easily isolated from the bulk heroin matrix, after which they are subjected to reduction with lithium aluminum hydride (LiAlH4) followed by derivatization with heptafluorobutyric anhydride (HFBA) in the presence of pyridine.The resultant haptafluorobutyryl (HFB) electrophiles are detected on-column at picogram (pg) levels by using capillary column gas chromatography/electron capture detection (CC/GC/ECD) in the splitless mode.The method is applicable for the in-depth analyses of crudely processed and highly refined heroin samples.