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Kenji Kuwayama et al.

Comparison and classification of methamphetamine seized in Japan and Thailand using gas chromatography with liquid-liquid extraction and solid-phase microextraction. Kenji Kuwayama et al. Present by. Lt.Sirikanya Ruangsri. 51312326. RESUME. NAME :. Lt.Sirikanya Ruangsri.

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Kenji Kuwayama et al.

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  1. Comparison and classification of methamphetamine seized in Japan and Thailand using gas chromatography with liquid-liquid extraction and solid-phase microextraction Kenji Kuwayama et al. Present by Lt.Sirikanya Ruangsri 51312326

  2. RESUME NAME : Lt.Sirikanya Ruangsri WORK EXPERIENCE : 2006- present : Scientific Crime Detection Division as Scientist 2004-2006 : The Partment Mineral Resource as Scientist Supachai Supalaknari, Ph.D. ADVISOR :

  3. INTRODUCTION

  4. Methamphetamine Caffeine Amphetamine

  5. Methamphetamine Amphetamine

  6. Receive eat inject smoke inhale

  7. Methamphetamine Ephedrine compound 1-phenyl-2-propanone (P2P) Synthesis : Methamphetamine

  8. ANALYSIS OF DRUG Presumptive Test Thin Layer Chromatography (TLC) Gas Chromatography Flame Ionization Detector (GC-FID) Gas Chromatography Mass Spectrometry (GC-MS) High Performance Liquid Chromatography (HPLC) Fourier Transform Infrared (FTIR) Spectroscopy ที่มา : United Nations Office on Drugs and Crime

  9. Two GC method for MA impurity profiling ONCB NRIPS Thenational Research Intitute of Police Science The Office of the Narcotics Control Board JAPAN THAILAND

  10. JAPAN THAI LLE

  11. Chromatograms obtained using the ONCB method tablet THAI crystal

  12. Chromatograms obtained from an MA crystal ONCB NRIPS

  13. The aim of this study • Improve the analytical method for profiling MA impurity • Compare and classification MA crystals seized in different countries • Information in criminal investigation ; traffic routes , the source of supply and relationships between seizures

  14. Method Liquid-Liquid Extraction ( LLE ) Solid-Phase Microextraction (SPME ) GC-FID & GC-MS

  15. Technique LLE solution sample Shaking centrifuge GC Organic layer 15

  16. TechniqueSPME SPME fiber Head space SPME fiber GC

  17. TechniqueGC-FID FID

  18. Technique GC-MS

  19. MATERIALS AND METHODS

  20. Reagents and chemical 1. MA.HCl crystals seized in Japan (69) and Thailand (42) 2. Std. d-MA.HCl 3. l-ephedrine.HCl 4. dl-Dimethylamphetamine.HCl 5. cis-1,2-dimethyl-3-phenylaziridine 6. n-Alkanes : Internal Standard 7. Solvents 8. SPME holder and fiber coated with DVB/CAR/PDMS 9. Inlet liner for SPME

  21. Gas chromatographic analysis 1.GC-FID Agilent – 6890 Auto inject :7683

  22. 2.GC-MS Agilent – 6890 Agilent 5973N MSD

  23. COLUMN GC-FID & GC-MS DB-5 capillary column ( 30 m. x 0.32 mm. xfilm thickness 1.0 µm. )

  24. LLE procedure ( NRIPS ) 0.5mL Ethyl acetate + Istd. buffer solution1 mL Shaking MA.HCl 50 mg Centrifuge 3000 rpm 5 min GC Istd.n-decane (C10,IS1) n-pentadecane (C15,IS2) n-eicosane (C20,IS3) n-octacosane (C28,IS4) 0.02 mg/ml 24

  25. SPME procedure Headspace at 85OC 35 min SPME fiber MA.HCl 10 mg SPME fiber GC

  26. Condition: GC-FID & GC-MS Initial temperature : 50 0C held 1 min. increase of 10 0C/min. to 300 0Cheld 10 min. Inject temperature : 240 0C Detector temperature : 300 0C Carrier gas : He(g) flow rate 2 mL / min. Injection : 1 µL splitless mode Condition for SPME were the same as those for LLE

  27. RESULTS

  28. Data processing for LLE & SPME • Peak data integrated by Chemstation software • Processed using the Drug Micro-Component Analysis & Comparison System (DMCPS) Calculation of Euclidean distances Cluster analysis by Ward method

  29. Data processing for LLE Istd.

  30. Typical chromatograms obtained from MA crystal using NRIPS Istd. Ephedrine (pseudoephedrine)

  31. Data processing for SPME

  32. Typical chromatograms obtained samples by SPME Empty vial without MA

  33. Typical chromatograms obtained samples by SPME

  34. 1.Optimization of analytical procedure LLE ONCB optimized for the analyzed of MA tablet NRIPS optimized for the analyzed of MA crystal considered more efficient than the ONCB

  35. 2.Cluster analysis of sample seized in Japan and Thailand Japan = 69 sample MA crystals seized Thai = 42 sample NRIPS method Cluster analysis Fourteen characteristic impurity peak

  36. 2.Cluster analysis of sample seized in Japan and Thailand NRIPS method 15/19 No.sam. (J/T) 25/0 17/15 12/8

  37. Typical chromatograms of MA samples in each group using the NRIPS High purity Group A Group B 1,3-dimethyl-2-phenyl naphthalene 1-benzyl-3-methylnaphthalene

  38. Typical chromatograms of MA samples in each group using the NRIPS cis-1,2-dimethyl-3-phenylaziridine Group C Ephedrine (pseudoephedrine) Group D

  39. 3.Comparison and classification of sample in the high purity group by SPME When MA crystals were extracted with SPME and analyzed by GC (SPME ), the chromatograms had many impurities while the chromatograms in case of LLE had few impurities Characteristic peaks for data processing seven peaks MA Many impurity

  40. 3.Comparison and classification of sample in the high purity group by SPME 15/19 SPME NRIPS

  41. 3.Comparison and classification of sample in the high purity group by SPME Chromatograms were distinguished clearlyfrom SPME method , whereas in the case of LLE it was difficult to compare and classify samples in the high-puritygroupbecause there were so few impurities. The SPME method enables us to compare and classify high-purity MA

  42. CONCLUSION

  43. ONCB Compared LLE Superior for detecting and separating MA impurities NRIPS 14 peaks characteristic Classified into four groups

  44. LLE SPME Effective for comparing high-purity MA because it detected many characteristic peaks

  45. THANKS FOR YOUR ATTENTION

  46. QUESTION

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