Determination of heroin and basic impurities for drug profiling by ultra-high-pressure liquid chromatography.

Rapid, precise, accurate, and reproducible methodology using ultra-high-pressure liquid chromatography (UHPLC) for the analysis of heroin and basic impurities is described. The determination of heroin, morphine, O3-monoacetylmorphine, O6-monoacetylmorphine, codeine, acetylcodeine, noscapine, and papaverine is accomplished using reversed-phase chromatography (RPC), employing a 1.7 µm Acquity UPLC BEH C18 column (2.1 mm × 150 mm) with a phosphate buffer (pH 1.6)-acetonitrile gradient and PDA detection. The target analytes are well resolved from each other and most adulterants in less than 20 min. For the few instances when adulterants interfere with target analytes, a 1.7 µm Acquity CSH Fluoro-Phenyl (2.1 mm × 150 mm) column is utilized with the same gradient conditions. The reported methodology can detect impurities as low as 0.02% relative to heroin, and is well suited for heroin profiling.

Stable isotope analyses of heroin seized from the merchant vessel Pong Su.

A new type of heroin HCl seized in Australia was examined by stable isotope analysis. The final origin/process classification of these samples by chromatographic signature profiles of the impurity/manufacturing by-products was previously determined to be "unknown" by two independent national laboratories. Various drug enforcement authorities speculated that the heroin might be from a new region or new illicit process due to the unusual chromatographic impurity profiles that were present. Samples from 20 different kilogram packages were examined for isotopic content to determine if the samples fit isotopic patterns of known origins or if they were unique to any known origins. Authentic specimens from Southeast Asian (N=59), Southwest Asia (N=37), South America (N=104), and Mexico (N=21) we concomitantly examined for comparison purposes. Both continuous flow elemental analysis-isotope ratio mass spectrometry and gas chromatography-isotope ratio mass spectrometry techniques were utilized. Heroin samples were also converted to morphine, without apparent isotopic fractionation, utilizing methanolic HCl for gas chromatography-isotope ratio mass spectrometry. The Pong Su samples were found to be isotopically and isotopically/alkaloidally distinct from the known origin/process classifications of Southwest Asian, Southeast Asian, South American, and Mexican.