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F Sporkert, F Pragst  Forensic Science International 

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Presentation on theme: "F Sporkert, F Pragst  Forensic Science International "— Presentation transcript:

1 Use of headspace solid-phase microextraction (HS-SPME) in hair analysis for organic compounds 
F Sporkert, F Pragst  Forensic Science International  Volume 107, Issue 1, Pages (January 2000) DOI: /S (99)

2 Fig. 1 Principle of headspace solid phase microextraction (HS-SPME) in hair analysis. Forensic Science International  , DOI: ( /S (99) )

3 Fig. 2 Effect of the reagents used for hair digestion and HS-SPME on the GC/MS abundance of the local anaesthetics lidocaine, propipocaine and etidocaine. HS-SPME conditions: fiber carbowax–DVB 65 μm, adsorption: 15 min at 70°C, m/e-values measured in GC/MS-SIM: propipocaine 121, 163 and 178, lidocaine 86 and 234, etidocaine 86, 128, 247. Forensic Science International  , DOI: ( /S (99) )

4 Fig. 3 Effect of the hair sample amount on the GC/MS peak area of some drugs after HS-SPME from 1 ml 4% NaOH+0.5 g Na2SO4. All samples were spiked with 50 ng of each drug. 100%=peak area in absence of hair. HS-SPME conditions: fiber PA 85 μm, adsorption 15 min at 70°C. Forensic Science International  , DOI: ( /S (99) )

5 Fig. 4 Effect of adsorption temperature on the GC/MS-SIM abundance in HS-SPME sample preparation. (A) Lidocaine with etidocaine as internal standard, fiber 65 μm Carbowax–DVB, adsorption time 15 min. (B) Amitriptyline with dimetacrine as internal standard, fiber 85 μm PA, adsorption time 15 min. Forensic Science International  , DOI: ( /S (99) )

6 Fig. 5 Effect of adsorption time on the GC/MS-SIM abundance in HS-SPME sample preparation. (A) Lidocaine with etidocaine as internal standard, fiber 65 μm Carbowax–DVB, adsorption temperature 70°C. (B) Amitriptyline with dimetacrine as internal standard, fiber 85 μm PA, adsorption temperature 90°C. Forensic Science International  , DOI: ( /S (99) )

7 Fig. 6 GC/MS-SIM chromatogram of a 10-mg hair sample (non-smoker) spiked with 16 drugs after HS-SPME sample preparation. Concentrations: 1 ng/mg, ethylbenzhydramine (peak 11, internal standard) 10 ng/mg, nicotine not added. Fiber: PA 85 μm. Adsorption: 15 min at 70°C. SIM measurement in nine time windows using the masses given in Table 1. Forensic Science International  , DOI: ( /S (99) )

8 Fig. 7 GC/MS-SIM chromatogram of the hair samples of a smoker and a passive smoker after HS-SPME with N,N-diethylaniline (100 ng/mg) as internal standard. m/z values cf. Table 1. Forensic Science International  , DOI: ( /S (99) )

9 Fig. 8 Hair concentrations of lidocaine in 49 drug fatalities determined by HS-SPME and GC/MS with etidocaine as internal standard [16]. HS-SPME conditions: fiber 65 μm Carbowax–DVB, adsorption 15 min at 70°C. Forensic Science International  , DOI: ( /S (99) )

10 Fig. 9 GC/MS-SIM chromatograms of some drugs from hair after sample preparation by alkaline hydrolysis and HS-SPME. Sample amount: 10 mg; internal standards: ethylbenzhydramine (A and B, 10 ng/mg) or D9-methadone (C, 10 ng/mg); fiber: PA 85 μm, adsorption 20 min at 80°C (A and C) or at 90°C (B), m/z values used in SIM see Table 1. (A) Subject (T098/97) with frequent intake of diphenhydramine. (B) Subject (T035/96) with frequent intake of tramadol. (C) Subject (T264/97) with regular intake of methadone. Forensic Science International  , DOI: ( /S (99) )

11 Fig. 10 GC/MS-SIM chromatograms of tricyclic antidepressants from hair after sample preparation by alkaline hydrolysis and HS-SPME. Sample amount: 10 mg; internal standard: dimetacrine (10 ng/mg); fiber: PA 85 μm, adsorption 20 min at 90°C, m/z values used in SIM see Table 1. (A) Subject (T164/99) with regular intake of amitriptyline and trimipramine. (B) Subject (T149/99) with regular intake of doxepine. Forensic Science International  , DOI: ( /S (99) )

12 Fig. 11 Detection of cannabinoids by HS-SPME and GC/MS-SIM. (A) 200 ng of cannabidiol, Δ9-tetrahydrocannabinol (THC) and cannabinol in 1 ml 4% NaOH after addition of 50 μl 85% H3PO4. (B) 30 mg hair of a cannabis consumer after 30 min hydrolysis in 1 ml 4% NaOH at 100°C and addition of 50 μl 85% H3PO4. Forensic Science International  , DOI: ( /S (99) )

13 Fig. 12 GC/MS-SIM chromatogram of the hair sample (10 mg) of an alcoholic with regular clomethiazole intake. Sample preparation: 12 h extraction in an ultrasonic bath with 1 ml buffer pH 6.0, subsequent addition of 0.5 g Na2SO4 and HS-SPME. Internal standard: N,N-diethylaniline (10 ng/mg); fiber: PA 85 μm, adsorption 15 min at 60°C, m/z values used in SIM cf. Table 1. Forensic Science International  , DOI: ( /S (99) )


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