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Aminoindanes

Chemical characterisation of aminoindan (e) products purchased from the Internet Jacqueline L. Stair Senior lecturer in analytical chemistry Centre for Clinical Practice, Safe Medicines and Drug Misuse Research. Aminoindanes. Aminoindanes.

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Aminoindanes

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  1. Chemical characterisation of aminoindan(e) products purchased from the InternetJacqueline L. StairSenior lecturer in analytical chemistryCentre for Clinical Practice, Safe Medicines and Drug Misuse Research

  2. Aminoindanes

  3. Aminoindanes • Full chemical characterisation of the pure substances by Casale et al. (2011; 2012) • Products often characterised as part of a diverse group • 19 products were analysed by Baron et al. (2012) • Primarily GC-MS analysis

  4. Assi, S.; Fergus, S.; Halsey, S.; Stair, J.L. “On-spot identification of so-called ‘legal highs’ using handheld Raman spectroscopy”. The Ever-Changing World of Psychoactive Drugs, Budapest, March 2012.

  5. overview • METHOD 1: Identification of volatile molecular constituents using Gas Chromatography Mass Spectrometry (GC-MS) • METHOD 2: Determination of non-volatile molecular constituents and quantification using Liquid Chromatography Photo Diode Array (LC-PDA) • METHOD 3: Identification and quantification of elemental constituents using Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES)

  6. aminoindanE products

  7. Method 1: Volatile molecular constituents GC Temperature Programme 0.1 mg/ml solutions prepared in methanol Analysed using Varian 450 GC/240 MS Varian FactorFour 5% phenyl-methyl capillary column (30m × 0.25mm × 0.25µm)

  8. methiopropamine (MPA) methylphenidate • Findings: • 6 products matched their label claim • Only 1-2 substances were detected • No 5-IAI was detected • 5 samples contained 2-AI Label: MDAI MPA Label:Aminoindan Caffeine Cola Vera Aminoacid Complex

  9. Method 2: NON-Volatile molecular constituents HPLC Gradient Method 0.5 mg/ml solutions prepared in methanol:water (50/50 v/v) Analysed using Perkin Elmer Flexar with PDA (λ=210 nm, FR=1.5 ml min-1) Phenomenex core Kinetex 5µ XB C18 column (150 × 4.6 mm)

  10. LC Method development CAF 2-AI 5-IAI MDAI Chromatogram of 2-AI, 5-IAI, MDAI, & CAF (0.5 mg/ml) using Kinetex XB-C18.

  11. Findings: • HPLC work confirmed number of constituents found by GC-MS. • Aminoindanes: • 11-84 %w/w • Caffeine: • 12-25 %w/w • Results indicate inorganic additives may be present

  12. Method 3:Elemental Constituents • ICP Torch 0.1 g used for each analysis Samples digested using conc. HNO3 and MW. Samples diluted and filtered Analysed using Varian ICP-OES with radial torch position.

  13. Which elements are present? • Semi-Quant analysis of all samples

  14. Which elements are present? • Semi-Quant analysis of all samples

  15. Calcium and magnesium Ca Mg

  16. selected Metals

  17. Lead ICH.Draft consensus guideline for elemental impurities Q3DCurrent Step 2b version. 26 July 2013.

  18. conclusions • For the products analysed, 6 out of 11 matched their label claim and no 5-IAI was detected. • Quantitative analysis showed concentration of aminoindanes ranged from 11-84 %w/w. • Elemental analysis using ICP-OES detected a range of constituents, but further work is needed.

  19. Acknowledgements Katy Kellett Dr. Jade D. Owen (Melbourne Scientific) Dr. SulafAssi (University of Bournemouth) Dr. Suzanne Fergus Dr. Mark Scott Prof. FabrizioSchifano SheelaghHalsey(Thermo Scientific) University of Hertfordshire

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