V T METHODS FOR IMPURITY PROFILING OF HEROIN AND COCAINE MANUAL FOR USE BY NATIONAL DRUG TESTING LABORATORIES Laboratory and Scientific Section United Nations Office on Drugs and Crime Vienna METHODS FOR IMPURITY PROFILING OF HEROIN AND COCAINE MANUAL FOR USE BY NATIONAL DRUG TESTING LABORATORIES UNITED NATIONS New York, 2005 Note Operating and experimental conditions are reproduced from the original reference materials. A number of alternative conditions and substitution of named commer- cial products may provide comparable results in many cases. Mention of names of firms and commercial products does not imply the endorsement of the United Nations. ST/NAR/35 UNITED NATIONS PUBLICATION Sales No. E.05.XI.14 ISBN 92-1-148206-2 Acknowledgements The Laboratory and Scientific Section of the United Nations Office on Drugs and Crime (UNODC) wishes to express its thanks to the following experts who par- ticipated in the Consultative Meeting on Recommended Methods for the Impurity Profiling of Heroin and Cocaine, organized by UNODC, in collaboration with the Australian Government Analytical Laboratories, in Sydney, Australia, from 8 to 12 November 1999, for their contribution to the contents of the present manual: Mr. Olivier Guéniat, Police de sûreté, Neuchâtel, Switzerland Mr. Adrian V. Kemmenoe, Forensic Science Service (FSS), Birmingham Laboratory, Birmingham, United Kingdom of Great Britain and Northern Ireland Mr. Helmut Neumann, Kriminaltechnisches Institut, Bundeskriminalamt (BKA), Wiesbaden, Germany Ms. Jana Skopec,* Australian Government Analytical Laboratories (AGAL), Pymble, New South Wales, Australia Mr. James Wong, Bureau of Drug Analysis Services (BDAS), Health Canada, Western Region Health Protection Branch, Burnaby, British Columbia, Canada The Laboratory and Scientific Section also wishes to express its thanks to Mr. Don Cooper and Mr. Helmut Neumann for reviewing, updating and finaliz- ing the manuscript, also using additional contributions from the participants.** *Now with Agrifor Scientific Pty Ltd., Australia. **Contact details of named individuals can be requested from the UNODC Laboratory and Scientific Section (P.O. Box 500, 1400 Vienna, Austria). iii Contents page I. Introduction. 1 A. Background . 1 B. Purpose of the manual. 2 C. Use of the manual . 3 II. Aspects of drug characterization and impurity profiling . 5 A. Background, concepts, purpose and strategies. 5 B. Analytical implications of heroin and cocaine manufacture and supply . 6 1. Determination of origin . 6 2. Establishing trafficking and distribution networks . 9 C. Types and investigational value of sample components . 10 1. Major components. 11 2. Trace components . 11 3. Residual and/or occluded solvents . 11 4. Trace elements . 12 5. Isotopic abundance . 12 III. Methods for impurity profiling . 13 A. General comments . 13 B. Heroin methods . 14 1. Hydrolysis of heroin . 14 2. Methods for the determination of major components . 16 3. Methods for the determination of trace components . 25 4. Residual solvent analysis . 31 5. Additional methods . 34 C. Cocaine methods . 35 1. Methods for the determination of major components. 36 2. Methods for the determination of trace components . 39 3. Residual solvent analysis . 44 4. Additional methods . 45 IV. Data handling, interpretation of results and approach to setting up profiling data collections . 47 A. Data handling. 47 B. Interpretation of results . 49 C. Approach to setting up profiling data collections . 49 v Annexes . 55 I. Supplementary information (for both heroin and cocaine) . 55 II. Impurities in heroin and cocaine and their “sources” . 57 III. Reference chromatograms and peak identification tables . 63 Bibliography . 75 vi I. INTRODUCTION A. Background In order to successfully counter the ever-growing drug problem, there is an increas- ing need, inter alia, to identify conspiracy links and trafficking routes and to gather background intelligence concerning both the number of sources of drugs and whether those sources are within a country or are “internationally” based and also the points of distribution and distribution networks. A scientific tool to complement routine law enforcement investigative work in this field is the characterization and impurity profiling of seized drugs. Drug characterization studies have shown that it is possible to link samples, to classify material from different seizures into groups of related samples and to identify the origin of samples. Such information can be used for evidential (judicial, court) purposes or it can be used as a source of intelligence to identify samples that may have a common origin or history. Drug characterization and impurity profiling may also assist in the identification of output from new illicit laboratories and in the monitoring of common methods used for drug manufacture, which, in turn, may provide information helpful to the maintenance of other intelligence- gathering tools, for example, precursor-monitoring programmes. Finally, drug characterization and impurity profiling may also provide supporting evidence in cases where illicitly manufactured drugs need to be differentiated from those diverted from licit sources. Beyond areas for application in the law enforcement and regulatory field, more in-depth analysis of drug samples, such as in drug characterization and impu- rity profiling studies, can also generate information essential for health authori- ties. The identification of unusual new drugs or drug combinations, for example, is a key element of early warning systems concerning unexpected adverse health consequences. Finally, systematic analysis of the composition of seized drugs also contributes to improved understanding of drug abuse trends. The laboratory of the United Nations Office on Drugs and Crime (UNODC) has a long history of involvement in drug characterization and impurity profiling. Opium characterization studies were initiated in 1948 and such study was one of the first and most comprehensive research efforts in international drug control under the aegis of the United Nations. In the late 1960s, the increasing abuse of heroin resulted in a shift in focus from opium to heroin. Pursuant to a request by the Commission on Narcotic Drugs, an expert group to determine the feasibility of using chemical characteristics for identifying sources and distribution patterns of heroin was convened in 1977 [1]. A follow-up meeting was held in Vienna in 1 2 Methods for impurity profiling of heroin and cocaine 1982 to coordinate research on the physical and chemical characteristics of heroin for the purpose of tracing origin and movement in the illicit traffic [2]. In 1992, a consultative meeting on chemical characterization and impurity profiling of drug seizures was held in Vienna; that meeting expanded coverage beyond heroin to include cocaine and synthetic drugs and, in particular, amphetamine [3]. At its thirty-ninth session, in 1996, the Commission on Narcotic Drugs rec- ognized the need for a cohesive international strategy in the field of drug char- acterization and impurity profiling. In so doing the Commission requested the Executive Director of the United Nations International Drug Control Programme (now called UNODC) to develop standard protocols and methods for the profil- ing/ signature analysis of key narcotic drugs and psychotropic substances [4]. The objectives of the Office in this area are to develop guidelines for characterization and impurity profiling of key narcotic drugs and psychotropic substances and to make the guidelines available to national forensic laboratories with the aim of providing them with a scientific tool to support law enforcement work for both evidential and strategic intelligence purposes. At the same time, the UNODC ref- erence services, which include the provision of training, reference samples, mate- rial and scientific literature, were expanded to include specific aspects of drug characterization and impurity profiling as well. In this context and in view of the focus of the General Assembly at its twen- tieth special session on, inter alia, the need for enhanced measures to counter illicit manufacture of and trafficking in drugs, it was considered timely to review profiling methods for heroin and cocaine, along with the broader concepts of drug characterization and impurity profiling of both plant-based and synthetic drugs. To this end, the Laboratory and Scientific Section of UNODC convened a Consultative Meeting on Recommended Methods for the Impurity Profiling of Heroin and Cocaine, in cooperation with the Government of Australia, in Sydney, Australia, in November 1999. B. Purpose of the manual The present manual, prepared by the Laboratory and Scientific Section of UNODC, reflects the discussions and conclusions of the Consultative Meeting held in Sydney. It is aimed at providing practical guidance to national drug test- ing laboratories that want to embark on heroin and/or cocaine profiling activities. The broader aspects of how drug characterization and impurity profiling can be used effectively as a scientific tool to support law enforcement operational inves- tigative work can be found in a separate manual entitled Drug Characterization/ Impurity Profiling: Background and Concepts [5], which was endorsed by the par- ticipants at the Consultative Meeting. Both manuals form part of a series of pub- lications dealing with the identification and analysis of various groups of drugs under international control. Specifically, the present manual complements United Nations