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  • Identification of impurities and the statistical classification of methamphetamine using headspace solid phase microextraction and gas chromatography-mass spectrometry.

Identification of impurities and the statistical classification of methamphetamine using headspace solid phase microextraction and gas chromatography-mass spectrometry.

Forensic science international (2005-09-29)
Kenji Kuwayama, Kenji Tsujikawa, Hajime Miyaguchi, Tatsuyuki Kanamori, Yuko Iwata, Hiroyuki Inoue, Shuji Saitoh, Tohru Kishi
ZUSAMMENFASSUNG

The profiling of impurities in methamphetamine (MA) using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) is described. The extraction of the impurities with an SPME fiber was examined under varying conditions. Optimal chromatograms were obtained when a 50 mg MA sample at 85 degrees C for 30 min was extracted using a fiber coated with divinylbenzene/carboxen/polydimethylsiloxane. MA samples from nine different origins were analyzed under optimized extraction conditions. Compounds related to MA such as benzaldehyde, benzyl alcohol, amphetamine, benzyl methyl ketone, cis- and trans-1,2-dimethyl-3-phenylaziridine, dimethylamphetamine, N-acetylamphetamine, N-acetylmethamphetamine and N-formylmethamphetamine were detected in the chromatograms. Trace amounts of ethanol, diethyl ether and acetic acid were also detected in some of the chromatograms. The numbers and intensities of the peaks detected were different, depending on the sample. After the areas of the eight principal peaks were converted to their square root and logarithm, similarities among the samples were evaluated by Euclidian distance, cosine distance and correlation coefficient. The results showed that a combination of logarithmic conversion and cosine distance was the most suitable for discriminating and classifying the samples. HS-SPME/GC-MS is a simple and effective method for the extraction and identification of impurities. The present method, in combination with an appropriate statistical analysis, would be useful for developing a profile of impurities in MA.

MATERIALIEN
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Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, plain gray hub
Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 24 ga, Autosampler, pk of 3, notched gray hub
Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, StableFlex (1cm), needle size 24 ga, Manual Holder, pk of 3, plain gray hub
Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 23 ga, Autosampler, pk of 3, notched gray hub
Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Autosampler, pk of 3, plain gray hub
Supelco
ORBO Carboxen-564 Röhrchen, W,F,F separators, O.D. × L 6 mm × 75 mm, pkg of 25 ea, for analyte group MEK (methylethyl ketone)
Supelco
ORBO 78 HBr auf Carboxen® 564 speziell gereinigt (20/45), 400/200 mg, W,W,W separators, O.D. × L 6 mm × 110 mm, pkg of 25 ea
Supelco
Carboxen®-1010 PLOT Kapillar-GC-Säule, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
Carboxen® Adsorptionsmittel, matrix Carboxen® 1000, 60-80 mesh, bottle of 10 g
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, black hub
Supelco
Carboxen®-1006 PLOT Kapillar-GC-Säule, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, black hub
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), 85 μm CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, light blue hub
Supelco
Carboxen®-1010 PLOT Kapillar-GC-Säule, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), 85 μm CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Manual Holder, pk of 3, light blue hub
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), 85 μm CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Autosampler, pk of 3, light blue hub
Supelco
ORBO-93 Sorbensröhrchen, ORBO tube I.D. × L 6 mm × 95 mm, Bed A 180 mg, Bed B 90 mg, 60/80 mesh, pkg of 25 ea
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 23 ga, Autosampler, pk of 3, black hub
Supelco
Carboxen®-1006 PLOT Kapillar-GC-Säule, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 23 ga, Manual Holder, pk of 3, black hub
Supelco
Tenax® TA / Carboxen® 1018, glass TD tube, preconditioned, O.D. × L 1/4 in. × 3 1/2 in., Sealed with (Swagelok® End-Fittings), pkg of 10 ea
Supelco
Carboxen® Adsorptionsmittel, matrix Carboxen® 1003, 40-60 mesh, bottle of 10 g
Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, Metal Alloy (2cm), needle size 23 ga, Autosampler, pk of 1, plain gray hub
Supelco
Carboxen® 572 for Tobacco Smoke, Adsorbent Bed Wt: 300 mg, cartridge size 3 mL, pkg of 50 ea
Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, Metal Alloy (1cm), needle size 23 ga, Autosampler, pk of, plain gray hub
Supelco
Carboxen® Adsorptionsmittel, matrix Carboxen® 569, 20-45 mesh, bottle of 10 g
Supelco
Carboxen® 1000 Reversibles SPE-Röhrchen, 200 mg/mL, pk 30
Supelco
Carboxen® Adsorptionsmittel, matrix Carboxen® 572, 20-45 mesh, bottle of 10 g
Supelco
Carboxen® Adsorptionsmittel, matrix Carboxen® 1000, 40-60 mesh, bottle of 50 g
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), 85 μm CAR/PDMS, Metal Alloy (1 cm), needle size 23 ga, Autosampler, pk of 1, light blue hub