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MICROCRYSTALLINE TESTS in FORENSIC DRUG ANALYSIS 3 Different Principles: E.G

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MICROCRYSTALLINE TESTS in FORENSIC DRUG ANALYSIS 3 Different Principles: E.G chromatography). Finally, the drug is systematically Microcrystalline Tests in quantified (e.g. mass spectrometry). Microcrystalline tests Forensic Drug Analysis fall within the second step of this analytical process. They are low cost because of the minute amount of reagents used and the simplicity of the instrumentation and consumables Mathieu P. Elie and Leonie E. Elie required to perform the analysis. They offer all the features School of Natural and Applied Sciences, University required by a good confirmation technique while being of Lincoln, Lincoln, UK very fast to administer and interpret, although they do not offer quantification capabilities. Microcrystalline tests are chemical tests resulting in the 1 Introduction 1 formation of unique microcrystals for a given substance 1.1 History 2 when combined with a specific reagent. Microcrystals are observed under a microscope and micrographs or 1.2 Modern Use 2 microvideos constitute the results of the test. 2 Chemical and Forensic Context 2 Thanks to the chemical mechanism by which micro- 2.1 Microchemical Identification 2 crystals develop, microcrystalline tests can be applied 2.2 The Value of Microcrystalline Tests for to molecules of various sizes, shapes, charges, and with Forensic Drug Analysis 2 different functional groups, and can naturally distinguish 2.3 Type of Evidence Provided by between enantiomers. Microcrystalline Tests 3 3 Technical AspecT 4 3.1 General Principle of Microcrystalline 1 INTRODUCTION Tests 4 3.2 Sample and Reagent Preparation 4 Forensic drug analysis is a vast field that involves the 3.3 Crystal Growth 5 application of a range of analytical techniques to identify 3.4 Crystal Classification and Description 6 and quantify drugs of abuse, to support authorities during 3.5 Storage, Shelf Life, and Sample investigation proceedings. Abuse of drugs is a worldwide Recovery 8 health problem touching all layers of the population irrespective of age and socioeconomic background. 4 Application Examples 8 In 1961, an international treaty was signed: the Single 4.1 Cocaine 8 Convention on Narcotic Drugs (SCND), which prohibits 4.2 Diamorphine (Heroin) 9 the production and supply of specific drugs (or related 4.3 Methadone 9 drugs) except those under license for medical or research 4.4 γ -Hydroxybutyrate 9 purposes. The substances addressed by the SCND were 4.5 Ketamine 10 opiates, cocaine, and cannabis. In 1971, the Convention 4.6 Phencyclidine 10 on Psychotropic Substances (CPS) added lysergic acid diethylamide (LSD), Ecstasy, and other psychotropic 4.7 Amphetamines and Methamphetamine 10 drugs. Finally, the United Nations Convention Against Acknowledgments 12 Illicit Traffic in Narcotic Drugs and Psychotropic Abbreviations and Acronyms 12 Substances introduced regulations on precursors in 1988. Related Articles 12 The SCND offered a base to develop national References 12 regulations across the globe, for example, the Substance Control Act in the United States (1970) and the Misuse of Drugs Act in the United Kingdom (1971). Commonly abused substances regulated in these Drug detection in the forensic context requires numerous acts include opioids (morphine, heroin, codeine, and analytical techniques. Depending on locally adopted methadone), cocaine, amphetamine, methamphetamine, standard procedures, different techniques are used for 3,4-methylenedioxymethamphetamine (MDMA), canna- screening solid samples for potential illicit substances bis, benzodiazepines, γ -hydroxybutyrate (GHB), (e.g. Fourier transform infrared spectroscopy (FTIR)). A flunitrazepam, phencyclidine (PCP), and barbiturates. sample suspected of containing prohibited material passes Numerous analytical techniques exist to screen seized through another layer of techniques to confirm that the material for the presence of drugs and to quantify illegal substance is present and to identify it (e.g. liquid/gas any amount detected. In this analytical framework, the Encyclopedia of Analytical Chemistry, Online © 2006–2009 John Wiley & Sons, Ltd. This article is © 2009 John Wiley & Sons, Ltd. This article was published in the Encyclopedia of Analytical Chemistry in 2009 by John Wiley & Sons, Ltd. DOI: 10.1002/9780470027318.a9102 2 FORENSIC SCIENCE purpose of microcrystalline tests is to make a definite and 1.2 Modern Use final identification when a drug is present in a sample. It is difficult to assess how widely microcrystalline tests are now used for forensic drug analysis. On the basis of the 1.1 History small number of recent publications, research activity in the development of microcrystalline tests seems limited, In the early 1800’s chemists started to apply reagents and existing guides issued by the American Society for on drugs, pharmaceuticals and food stuffs and observed Testing and Materials (ASTM) describing such tests are reactions such as color changes through a microscope. outdated. With the development of the polarized light microscope, However, the recent emergence of GHB on the the observation of crystals evolved rapidly because it drug facilitated sexual assault (DFSA) scene has seen reveals local differences in specimen structures, although the sudden publication of three papers proposing it was mostly utilized for mineralogy.(1,2) microcrystalline tests for this drug.(8–10) In 1827, Raspail introduced the term ‘‘chemical Indeed, GHB being a very small (104.1 g mol−1) microscopy’’.(3) By then he had already discovered and simple molecule, finding a specific test for it microchemical tests for the detection of sugars, oils, was challenging. Nevertheless, GHB can be detected and albumin within cell material. In the middle of the effortlessly using a microcrystalline test, thanks to the nineteenth century, toxicologists started to study crystal technique mechanism. formations of alkaloids when combined with reagents, and the first crystal tests emerged. From then on, microcrystalline tests developed more systematically up to the publication of ‘‘Microchemistry of Poisons’’ by 2 CHEMICAL AND FORENSIC CONTEXT Wormley in 1867, which included microcrystal illustra- tions engraved upon steel.(4) 2.1 Microchemical Identification The technique evolved across inorganic and organic A microcrystalline test is a chemical test and the result is a chemistry from the simple use of a microscope to aid microcrystal observed under a microscope. After allowing chemical identification to the development of reactions the sample to meet with a carefully chosen reagent, testing that led to the formation of characteristic crystals. whether a drug is present using this technique relies on Fulton published the only textbook on microcrystalline comparing the shape, size, color, and spatial arrangement tests, which covers numerous microcrystalline tests for the (also called habit)(6) of the microcrystals formed with the identification of narcotics and drugs of abuse from simple those formed in a control with the same reagent. The test setup to result in the interpretation and development (5) control is an authentic sample of the drug tested for. If of new tests. This provided a detailed classification for the crystal’s shape, size, color, and spatial arrangements crystal characterization including numerous micropho- match, the analyst can conclude a positive identification tographs showing various shapes and appearances. of the drug. Clarke extended the range of microcrystalline tests mostly focusing on toxicology applications.(6) At a time when analytical techniques such as chromatography were 2.2 The Value of Microcrystalline Tests for Forensic evolving fast but could not yet routinely be used to Drug Analysis identify unknown drugs, reliable microchemical tests The microcrystalline test technique is often wrongly such as microcrystalline and color tests were needed classified as a screening technique and/or a presumptive and developed. technique. A microcrystalline test should be classified and After 1969, publications on microcrystalline tests for considered as a confirmation technique with screening drugs were based either on Fulton’s or on Clarke’s work capability. and only rarely contained new tests. A good confirmation technique must have three However, when modern separation and detection main qualities. First, the technique needs to present techniques, especially gas chromatography/mass spec- a certain predictive aspect where the results obtained trometry (GC/MS) and liquid chromatography/mass are expected. The confirmation technique is chosen spectrometry (LC/MS) became widely available and because of its specificity and sensitivity for the suspected reliable, techniques that did not provide any molec- substance. Second, the technique should consider the ular, structural, and/or compositional information were whole compound and not just its reactive groups. gradually neglected and eventually used as presump- Finally, a confirmation technique must be different, either tive/screening tests. Microcrystalline tests were entirely in its nature or its results, from any test previously removed from Clarke’s Isolation and Identification of used to screen and identify the substance. Different Drugs, second edition (1986).(7) analytical techniques base substance identification on Encyclopedia of Analytical Chemistry, Online © 2006–2009 John Wiley & Sons, Ltd. This article is © 2009 John Wiley & Sons, Ltd. This article was published in the Encyclopedia of Analytical Chemistry in 2009 by John Wiley & Sons, Ltd. DOI: 10.1002/9780470027318.a9102 MICROCRYSTALLINE TESTS IN FORENSIC DRUG ANALYSIS 3 different principles: e.g. retention
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