Chemical signature of ecstasy volatiles by comprehensive two-dimensional gas chromatography
Identifieur interne : 001B55 ( PascalFrancis/Corpus ); précédent : 001B54; suivant : 001B56Chemical signature of ecstasy volatiles by comprehensive two-dimensional gas chromatography
Auteurs : Blagoj Mitrevski ; Biljana Veleska ; Erwan Engel ; Paul Wynne ; SHIN MIIN SONG ; Philip J. MarriottSource :
- Forensic science international [ 0379-0738 ] ; 2011.
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- Pascal (Inist)
English descriptors
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Abstract
A method for ecstasy volatiles 'signature' analysis based on two-dimensional gas chromatography separation and time-of-flight mass spectrometry detection (GC x GC-TOFMS) is presented. Organic impurity volatiles were extracted by head space solid phase microextraction (HS-SPME). The final column phase choice of the four different column combinations tested was a low-polarity 5% phenyl polysilphenylene-siloxane coupled with a polyethylene glycol phase, which best displayed the complex impurity profile. Second dimension (2D) retention time reproducibility was found to be about 1 % RSD, and area reproducibility of SPME sampling was just over 5% RSD for compounds with S/N ratio of about 100. High similarity of TOFMS spectra of impurities was obtained against commercial MS libraries. 16 components from the two-dimensional profiles were selected for comparison of the 24 ecstasy tablets, most of which proved to be benzodioxole derived compounds. All tablets were correctly classified in eight groups according to their post-tabletting characteristics, when appropriate data pre-treatment was applied. Principal component analysis revealed clustering of samples according to the country of origin. Samples from Macedonia were elevated in N-formyl-MDMA and N-acetyl-MDMA while samples from Australia were elevated in 3,4-methylenedioxypropane and 3,4-methylenedioxyacetophenone. Furthermore, three components were found to be unique for one of the source countries. The additional separation of components on the 2D column, increased response due to modulation, high acquisition rate with full mass spectra using TOFMS detection, and MS deconvolution extend the possibility of detecting additional markers and route-specific components, especially of low abundant, polar components.
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Format Inist (serveur)
| NO : | PASCAL 11-0300963 INIST |
|---|---|
| ET : | Chemical signature of ecstasy volatiles by comprehensive two-dimensional gas chromatography |
| AU : | MITREVSKI (Blagoj); VELESKA (Biljana); ENGEL (Erwan); WYNNE (Paul); SHIN MIIN SONG; MARRIOTT (Philip J.) |
| AF : | Australian Centre for Research on Separation Science, RMIT University, GPO Box 2476V/Melbourne, Victoria 3001/Australie (1 aut., 3 aut., 6 aut.); Forensic Science Unit, Ministry of Internal Affairs, Dimce Mircev bb/1000 Skopje/Macédoine (2 aut.); INRA, UR370 QuaPA/63122 Saint-Genes-Champanelle/France (3 aut.); SGE Analytical Science Ltd., 7 Argent Place/Ringwood, Victoria 3134/Australie (4 aut.); Institute of Microelectronics, Agency for Science, Technology and Research (A*STAR), 11 Science Park Road/Singapore 117685/Singapour (5 aut.) |
| DT : | Publication en série; Niveau analytique |
| SO : | Forensic science international; ISSN 0379-0738; Coden FSINDR; Royaume-Uni; Da. 2011; Vol. 209; No. 1-3; Pp. 11-20; Bibl. 42 ref. |
| LA : | Anglais |
| EA : | A method for ecstasy volatiles 'signature' analysis based on two-dimensional gas chromatography separation and time-of-flight mass spectrometry detection (GC x GC-TOFMS) is presented. Organic impurity volatiles were extracted by head space solid phase microextraction (HS-SPME). The final column phase choice of the four different column combinations tested was a low-polarity 5% phenyl polysilphenylene-siloxane coupled with a polyethylene glycol phase, which best displayed the complex impurity profile. Second dimension (2D) retention time reproducibility was found to be about 1 % RSD, and area reproducibility of SPME sampling was just over 5% RSD for compounds with S/N ratio of about 100. High similarity of TOFMS spectra of impurities was obtained against commercial MS libraries. 16 components from the two-dimensional profiles were selected for comparison of the 24 ecstasy tablets, most of which proved to be benzodioxole derived compounds. All tablets were correctly classified in eight groups according to their post-tabletting characteristics, when appropriate data pre-treatment was applied. Principal component analysis revealed clustering of samples according to the country of origin. Samples from Macedonia were elevated in N-formyl-MDMA and N-acetyl-MDMA while samples from Australia were elevated in 3,4-methylenedioxypropane and 3,4-methylenedioxyacetophenone. Furthermore, three components were found to be unique for one of the source countries. The additional separation of components on the 2D column, increased response due to modulation, high acquisition rate with full mass spectra using TOFMS detection, and MS deconvolution extend the possibility of detecting additional markers and route-specific components, especially of low abundant, polar components. |
| CC : | 002B24; 002B30A10; 002B01 |
| FD : | Amphétamine(N-méthyl-3,4-méthylènedioxy); Substance toxicomanogène; Impureté; Chromatographie phase gazeuse; Criminalistique; Médecine légale; Aspect médicolégal; Police scientifique; Ecstasy; Profilage criminel |
| FG : | Drogue illicite; Drogue récréative |
| ED : | Drug of abuse; Impurity; Gas chromatography; Criminalistics; Legal medicine; Forensic aspect; Forensic science |
| EG : | Illicit drug; Recreational drug |
| SD : | Sustancia toxicomanógena; Impureza; Cromatografía fase gaseosa; Criminalistica; Medicina legal; Aspecto forense; Ciencia forense |
| LO : | INIST-15440.354000190377130020 |
| ID : | 11-0300963 |
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Pascal:11-0300963Le document en format XML
<record><TEI><teiHeader><fileDesc><titleStmt><title xml:lang="en" level="a">Chemical signature of ecstasy volatiles by comprehensive two-dimensional gas chromatography</title><author><name sortKey="Mitrevski, Blagoj" sort="Mitrevski, Blagoj" uniqKey="Mitrevski B" first="Blagoj" last="Mitrevski">Blagoj Mitrevski</name><affiliation><inist:fA14 i1="01"><s1>Australian Centre for Research on Separation Science, RMIT University, GPO Box 2476V</s1><s2>Melbourne, Victoria 3001</s2><s3>AUS</s3><sZ>1 aut.</sZ><sZ>3 aut.</sZ><sZ>6 aut.</sZ></inist:fA14></affiliation></author><author><name sortKey="Veleska, Biljana" sort="Veleska, Biljana" uniqKey="Veleska B" first="Biljana" last="Veleska">Biljana Veleska</name><affiliation><inist:fA14 i1="02"><s1>Forensic Science Unit, Ministry of Internal Affairs, Dimce Mircev bb</s1><s2>1000 Skopje</s2><s3>MKD</s3><sZ>2 aut.</sZ></inist:fA14></affiliation></author><author><name sortKey="Engel, Erwan" sort="Engel, Erwan" uniqKey="Engel E" first="Erwan" last="Engel">Erwan Engel</name><affiliation><inist:fA14 i1="01"><s1>Australian Centre for Research on Separation Science, RMIT University, GPO Box 2476V</s1><s2>Melbourne, Victoria 3001</s2><s3>AUS</s3><sZ>1 aut.</sZ><sZ>3 aut.</sZ><sZ>6 aut.</sZ></inist:fA14></affiliation><affiliation><inist:fA14 i1="03"><s1>INRA, UR370 QuaPA</s1><s2>63122 Saint-Genes-Champanelle</s2><s3>FRA</s3><sZ>3 aut.</sZ></inist:fA14></affiliation></author><author><name sortKey="Wynne, Paul" sort="Wynne, Paul" uniqKey="Wynne P" first="Paul" last="Wynne">Paul Wynne</name><affiliation><inist:fA14 i1="04"><s1>SGE Analytical Science Ltd., 7 Argent Place</s1><s2>Ringwood, Victoria 3134</s2><s3>AUS</s3><sZ>4 aut.</sZ></inist:fA14></affiliation></author><author><name sortKey="Shin Miin Song" sort="Shin Miin Song" uniqKey="Shin Miin Song" last="Shin Miin Song">SHIN MIIN SONG</name><affiliation><inist:fA14 i1="05"><s1>Institute of Microelectronics, Agency for Science, Technology and Research (A*STAR), 11 Science Park Road</s1><s2>Singapore 117685</s2><s3>SGP</s3><sZ>5 aut.</sZ></inist:fA14></affiliation></author><author><name sortKey="Marriott, Philip J" sort="Marriott, Philip J" uniqKey="Marriott P" first="Philip J." last="Marriott">Philip J. Marriott</name><affiliation><inist:fA14 i1="01"><s1>Australian Centre for Research on Separation Science, RMIT University, GPO Box 2476V</s1><s2>Melbourne, Victoria 3001</s2><s3>AUS</s3><sZ>1 aut.</sZ><sZ>3 aut.</sZ><sZ>6 aut.</sZ></inist:fA14></affiliation></author></titleStmt><publicationStmt><idno type="wicri:source">INIST</idno><idno type="inist">11-0300963</idno><date when="2011">2011</date><idno type="stanalyst">PASCAL 11-0300963 INIST</idno><idno type="RBID">Pascal:11-0300963</idno><idno type="wicri:Area/PascalFrancis/Corpus">001B55</idno></publicationStmt><sourceDesc><biblStruct><analytic><title xml:lang="en" level="a">Chemical signature of ecstasy volatiles by comprehensive two-dimensional gas chromatography</title><author><name sortKey="Mitrevski, Blagoj" sort="Mitrevski, Blagoj" uniqKey="Mitrevski B" first="Blagoj" last="Mitrevski">Blagoj Mitrevski</name><affiliation><inist:fA14 i1="01"><s1>Australian Centre for Research on Separation Science, RMIT University, GPO Box 2476V</s1><s2>Melbourne, Victoria 3001</s2><s3>AUS</s3><sZ>1 aut.</sZ><sZ>3 aut.</sZ><sZ>6 aut.</sZ></inist:fA14></affiliation></author><author><name sortKey="Veleska, Biljana" sort="Veleska, Biljana" uniqKey="Veleska B" first="Biljana" last="Veleska">Biljana Veleska</name><affiliation><inist:fA14 i1="02"><s1>Forensic Science Unit, Ministry of Internal Affairs, Dimce Mircev bb</s1><s2>1000 Skopje</s2><s3>MKD</s3><sZ>2 aut.</sZ></inist:fA14></affiliation></author><author><name sortKey="Engel, Erwan" sort="Engel, Erwan" uniqKey="Engel E" first="Erwan" last="Engel">Erwan Engel</name><affiliation><inist:fA14 i1="01"><s1>Australian Centre for Research on Separation Science, RMIT University, GPO Box 2476V</s1><s2>Melbourne, Victoria 3001</s2><s3>AUS</s3><sZ>1 aut.</sZ><sZ>3 aut.</sZ><sZ>6 aut.</sZ></inist:fA14></affiliation><affiliation><inist:fA14 i1="03"><s1>INRA, UR370 QuaPA</s1><s2>63122 Saint-Genes-Champanelle</s2><s3>FRA</s3><sZ>3 aut.</sZ></inist:fA14></affiliation></author><author><name sortKey="Wynne, Paul" sort="Wynne, Paul" uniqKey="Wynne P" first="Paul" last="Wynne">Paul Wynne</name><affiliation><inist:fA14 i1="04"><s1>SGE Analytical Science Ltd., 7 Argent Place</s1><s2>Ringwood, Victoria 3134</s2><s3>AUS</s3><sZ>4 aut.</sZ></inist:fA14></affiliation></author><author><name sortKey="Shin Miin Song" sort="Shin Miin Song" uniqKey="Shin Miin Song" last="Shin Miin Song">SHIN MIIN SONG</name><affiliation><inist:fA14 i1="05"><s1>Institute of Microelectronics, Agency for Science, Technology and Research (A*STAR), 11 Science Park Road</s1><s2>Singapore 117685</s2><s3>SGP</s3><sZ>5 aut.</sZ></inist:fA14></affiliation></author><author><name sortKey="Marriott, Philip J" sort="Marriott, Philip J" uniqKey="Marriott P" first="Philip J." last="Marriott">Philip J. Marriott</name><affiliation><inist:fA14 i1="01"><s1>Australian Centre for Research on Separation Science, RMIT University, GPO Box 2476V</s1><s2>Melbourne, Victoria 3001</s2><s3>AUS</s3><sZ>1 aut.</sZ><sZ>3 aut.</sZ><sZ>6 aut.</sZ></inist:fA14></affiliation></author></analytic><series><title level="j" type="main">Forensic science international</title><title level="j" type="abbreviated">Forensic sci. int.</title><idno type="ISSN">0379-0738</idno><imprint><date when="2011">2011</date></imprint></series></biblStruct></sourceDesc><seriesStmt><title level="j" type="main">Forensic science international</title><title level="j" type="abbreviated">Forensic sci. int.</title><idno type="ISSN">0379-0738</idno></seriesStmt></fileDesc><profileDesc><textClass><keywords scheme="KwdEn" xml:lang="en"><term>Criminalistics</term><term>Drug of abuse</term><term>Forensic aspect</term><term>Forensic science</term><term>Gas chromatography</term><term>Impurity</term><term>Legal medicine</term></keywords><keywords scheme="Pascal" xml:lang="fr"><term>Amphétamine(N-méthyl-3,4-méthylènedioxy)</term><term>Substance toxicomanogène</term><term>Impureté</term><term>Chromatographie phase gazeuse</term><term>Criminalistique</term><term>Médecine légale</term><term>Aspect médicolégal</term><term>Police scientifique</term><term>Ecstasy</term><term>Profilage criminel</term></keywords></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en">A method for ecstasy volatiles 'signature' analysis based on two-dimensional gas chromatography separation and time-of-flight mass spectrometry detection (GC x GC-TOFMS) is presented. Organic impurity volatiles were extracted by head space solid phase microextraction (HS-SPME). The final column phase choice of the four different column combinations tested was a low-polarity 5% phenyl polysilphenylene-siloxane coupled with a polyethylene glycol phase, which best displayed the complex impurity profile. Second dimension (<sup>2</sup>D) retention time reproducibility was found to be about 1 % RSD, and area reproducibility of SPME sampling was just over 5% RSD for compounds with S/N ratio of about 100. High similarity of TOFMS spectra of impurities was obtained against commercial MS libraries. 16 components from the two-dimensional profiles were selected for comparison of the 24 ecstasy tablets, most of which proved to be benzodioxole derived compounds. All tablets were correctly classified in eight groups according to their post-tabletting characteristics, when appropriate data pre-treatment was applied. Principal component analysis revealed clustering of samples according to the country of origin. Samples from Macedonia were elevated in N-formyl-MDMA and N-acetyl-MDMA while samples from Australia were elevated in 3,4-methylenedioxypropane and 3,4-methylenedioxyacetophenone. Furthermore, three components were found to be unique for one of the source countries. The additional separation of components on the <sup>2</sup>D column, increased response due to modulation, high acquisition rate with full mass spectra using TOFMS detection, and MS deconvolution extend the possibility of detecting additional markers and route-specific components, especially of low abundant, polar components.</div></front></TEI><inist><standard h6="B"><pA><fA01 i1="01" i2="1"><s0>0379-0738</s0></fA01><fA02 i1="01"><s0>FSINDR</s0></fA02><fA03 i2="1"><s0>Forensic sci. int.</s0></fA03><fA05><s2>209</s2></fA05><fA06><s2>1-3</s2></fA06><fA08 i1="01" i2="1" l="ENG"><s1>Chemical signature of ecstasy volatiles by comprehensive two-dimensional gas chromatography</s1></fA08><fA11 i1="01" i2="1"><s1>MITREVSKI (Blagoj)</s1></fA11><fA11 i1="02" i2="1"><s1>VELESKA (Biljana)</s1></fA11><fA11 i1="03" i2="1"><s1>ENGEL (Erwan)</s1></fA11><fA11 i1="04" i2="1"><s1>WYNNE (Paul)</s1></fA11><fA11 i1="05" i2="1"><s1>SHIN MIIN SONG</s1></fA11><fA11 i1="06" i2="1"><s1>MARRIOTT (Philip J.)</s1></fA11><fA14 i1="01"><s1>Australian Centre for Research on Separation Science, RMIT University, GPO Box 2476V</s1><s2>Melbourne, Victoria 3001</s2><s3>AUS</s3><sZ>1 aut.</sZ><sZ>3 aut.</sZ><sZ>6 aut.</sZ></fA14><fA14 i1="02"><s1>Forensic Science Unit, Ministry of Internal Affairs, Dimce Mircev bb</s1><s2>1000 Skopje</s2><s3>MKD</s3><sZ>2 aut.</sZ></fA14><fA14 i1="03"><s1>INRA, UR370 QuaPA</s1><s2>63122 Saint-Genes-Champanelle</s2><s3>FRA</s3><sZ>3 aut.</sZ></fA14><fA14 i1="04"><s1>SGE Analytical Science Ltd., 7 Argent Place</s1><s2>Ringwood, Victoria 3134</s2><s3>AUS</s3><sZ>4 aut.</sZ></fA14><fA14 i1="05"><s1>Institute of Microelectronics, Agency for Science, Technology and Research (A*STAR), 11 Science Park Road</s1><s2>Singapore 117685</s2><s3>SGP</s3><sZ>5 aut.</sZ></fA14><fA20><s1>11-20</s1></fA20><fA21><s1>2011</s1></fA21><fA23 i1="01"><s0>ENG</s0></fA23><fA43 i1="01"><s1>INIST</s1><s2>15440</s2><s5>354000190377130020</s5></fA43><fA44><s0>0000</s0><s1>© 2011 INIST-CNRS. All rights reserved.</s1></fA44><fA45><s0>42 ref.</s0></fA45><fA47 i1="01" i2="1"><s0>11-0300963</s0></fA47><fA60><s1>P</s1></fA60><fA61><s0>A</s0></fA61><fA64 i1="01" i2="1"><s0>Forensic science international</s0></fA64><fA66 i1="01"><s0>GBR</s0></fA66><fC01 i1="01" l="ENG"><s0>A method for ecstasy volatiles 'signature' analysis based on two-dimensional gas chromatography separation and time-of-flight mass spectrometry detection (GC x GC-TOFMS) is presented. Organic impurity volatiles were extracted by head space solid phase microextraction (HS-SPME). The final column phase choice of the four different column combinations tested was a low-polarity 5% phenyl polysilphenylene-siloxane coupled with a polyethylene glycol phase, which best displayed the complex impurity profile. Second dimension (<sup>2</sup>D) retention time reproducibility was found to be about 1 % RSD, and area reproducibility of SPME sampling was just over 5% RSD for compounds with S/N ratio of about 100. High similarity of TOFMS spectra of impurities was obtained against commercial MS libraries. 16 components from the two-dimensional profiles were selected for comparison of the 24 ecstasy tablets, most of which proved to be benzodioxole derived compounds. All tablets were correctly classified in eight groups according to their post-tabletting characteristics, when appropriate data pre-treatment was applied. Principal component analysis revealed clustering of samples according to the country of origin. Samples from Macedonia were elevated in N-formyl-MDMA and N-acetyl-MDMA while samples from Australia were elevated in 3,4-methylenedioxypropane and 3,4-methylenedioxyacetophenone. Furthermore, three components were found to be unique for one of the source countries. The additional separation of components on the <sup>2</sup>D column, increased response due to modulation, high acquisition rate with full mass spectra using TOFMS detection, and MS deconvolution extend the possibility of detecting additional markers and route-specific components, especially of low abundant, polar components.</s0></fC01><fC02 i1="01" i2="X"><s0>002B24</s0></fC02><fC02 i1="02" i2="X"><s0>002B30A10</s0></fC02><fC02 i1="03" i2="X"><s0>002B01</s0></fC02><fC03 i1="01" i2="X" l="FRE"><s0>Amphétamine(N-méthyl-3,4-méthylènedioxy)</s0><s2>FX</s2><s5>01</s5></fC03><fC03 i1="02" i2="X" l="FRE"><s0>Substance toxicomanogène</s0><s5>02</s5></fC03><fC03 i1="02" i2="X" l="ENG"><s0>Drug of abuse</s0><s5>02</s5></fC03><fC03 i1="02" i2="X" l="SPA"><s0>Sustancia toxicomanógena</s0><s5>02</s5></fC03><fC03 i1="03" i2="X" l="FRE"><s0>Impureté</s0><s5>03</s5></fC03><fC03 i1="03" i2="X" l="ENG"><s0>Impurity</s0><s5>03</s5></fC03><fC03 i1="03" i2="X" l="SPA"><s0>Impureza</s0><s5>03</s5></fC03><fC03 i1="04" i2="X" l="FRE"><s0>Chromatographie phase gazeuse</s0><s5>04</s5></fC03><fC03 i1="04" i2="X" l="ENG"><s0>Gas chromatography</s0><s5>04</s5></fC03><fC03 i1="04" i2="X" l="SPA"><s0>Cromatografía fase gaseosa</s0><s5>04</s5></fC03><fC03 i1="05" i2="X" l="FRE"><s0>Criminalistique</s0><s5>05</s5></fC03><fC03 i1="05" i2="X" l="ENG"><s0>Criminalistics</s0><s5>05</s5></fC03><fC03 i1="05" i2="X" l="SPA"><s0>Criminalistica</s0><s5>05</s5></fC03><fC03 i1="06" i2="X" l="FRE"><s0>Médecine légale</s0><s5>06</s5></fC03><fC03 i1="06" i2="X" l="ENG"><s0>Legal medicine</s0><s5>06</s5></fC03><fC03 i1="06" i2="X" l="SPA"><s0>Medicina legal</s0><s5>06</s5></fC03><fC03 i1="07" i2="X" l="FRE"><s0>Aspect médicolégal</s0><s5>25</s5></fC03><fC03 i1="07" i2="X" l="ENG"><s0>Forensic aspect</s0><s5>25</s5></fC03><fC03 i1="07" i2="X" l="SPA"><s0>Aspecto forense</s0><s5>25</s5></fC03><fC03 i1="08" i2="X" l="FRE"><s0>Police scientifique</s0><s5>26</s5></fC03><fC03 i1="08" i2="X" l="ENG"><s0>Forensic science</s0><s5>26</s5></fC03><fC03 i1="08" i2="X" l="SPA"><s0>Ciencia forense</s0><s5>26</s5></fC03><fC03 i1="09" i2="X" l="FRE"><s0>Ecstasy</s0><s4>INC</s4><s5>86</s5></fC03><fC03 i1="10" i2="X" l="FRE"><s0>Profilage criminel</s0><s4>INC</s4><s5>87</s5></fC03><fC07 i1="01" i2="X" l="FRE"><s0>Drogue illicite</s0><s5>37</s5></fC07><fC07 i1="01" i2="X" l="ENG"><s0>Illicit drug</s0><s5>37</s5></fC07><fC07 i1="01" i2="X" l="SPA"><s0>Droga ilícita</s0><s5>37</s5></fC07><fC07 i1="02" i2="X" l="FRE"><s0>Drogue récréative</s0><s2>FX</s2><s5>38</s5></fC07><fC07 i1="02" i2="X" l="ENG"><s0>Recreational drug</s0><s2>FX</s2><s5>38</s5></fC07><fC07 i1="02" i2="X" l="SPA"><s0>Droga recreativa</s0><s2>FX</s2><s5>38</s5></fC07><fN21><s1>206</s1></fN21><fN44 i1="01"><s1>OTO</s1></fN44><fN82><s1>OTO</s1></fN82></pA></standard><server><NO>PASCAL 11-0300963 INIST</NO><ET>Chemical signature of ecstasy volatiles by comprehensive two-dimensional gas chromatography</ET><AU>MITREVSKI (Blagoj); VELESKA (Biljana); ENGEL (Erwan); WYNNE (Paul); SHIN MIIN SONG; MARRIOTT (Philip J.)</AU><AF>Australian Centre for Research on Separation Science, RMIT University, GPO Box 2476V/Melbourne, Victoria 3001/Australie (1 aut., 3 aut., 6 aut.); Forensic Science Unit, Ministry of Internal Affairs, Dimce Mircev bb/1000 Skopje/Macédoine (2 aut.); INRA, UR370 QuaPA/63122 Saint-Genes-Champanelle/France (3 aut.); SGE Analytical Science Ltd., 7 Argent Place/Ringwood, Victoria 3134/Australie (4 aut.); Institute of Microelectronics, Agency for Science, Technology and Research (A*STAR), 11 Science Park Road/Singapore 117685/Singapour (5 aut.)</AF><DT>Publication en série; Niveau analytique</DT><SO>Forensic science international; ISSN 0379-0738; Coden FSINDR; Royaume-Uni; Da. 2011; Vol. 209; No. 1-3; Pp. 11-20; Bibl. 42 ref.</SO><LA>Anglais</LA><EA>A method for ecstasy volatiles 'signature' analysis based on two-dimensional gas chromatography separation and time-of-flight mass spectrometry detection (GC x GC-TOFMS) is presented. Organic impurity volatiles were extracted by head space solid phase microextraction (HS-SPME). The final column phase choice of the four different column combinations tested was a low-polarity 5% phenyl polysilphenylene-siloxane coupled with a polyethylene glycol phase, which best displayed the complex impurity profile. Second dimension (<sup>2</sup>D) retention time reproducibility was found to be about 1 % RSD, and area reproducibility of SPME sampling was just over 5% RSD for compounds with S/N ratio of about 100. High similarity of TOFMS spectra of impurities was obtained against commercial MS libraries. 16 components from the two-dimensional profiles were selected for comparison of the 24 ecstasy tablets, most of which proved to be benzodioxole derived compounds. All tablets were correctly classified in eight groups according to their post-tabletting characteristics, when appropriate data pre-treatment was applied. Principal component analysis revealed clustering of samples according to the country of origin. Samples from Macedonia were elevated in N-formyl-MDMA and N-acetyl-MDMA while samples from Australia were elevated in 3,4-methylenedioxypropane and 3,4-methylenedioxyacetophenone. Furthermore, three components were found to be unique for one of the source countries. The additional separation of components on the <sup>2</sup>D column, increased response due to modulation, high acquisition rate with full mass spectra using TOFMS detection, and MS deconvolution extend the possibility of detecting additional markers and route-specific components, especially of low abundant, polar components.</EA><CC>002B24; 002B30A10; 002B01</CC><FD>Amphétamine(N-méthyl-3,4-méthylènedioxy); Substance toxicomanogène; Impureté; Chromatographie phase gazeuse; Criminalistique; Médecine légale; Aspect médicolégal; Police scientifique; Ecstasy; Profilage criminel</FD><FG>Drogue illicite; Drogue récréative</FG><ED>Drug of abuse; Impurity; Gas chromatography; Criminalistics; Legal medicine; Forensic aspect; Forensic science</ED><EG>Illicit drug; Recreational drug</EG><SD>Sustancia toxicomanógena; Impureza; Cromatografía fase gaseosa; Criminalistica; Medicina legal; Aspecto forense; Ciencia forense</SD><LO>INIST-15440.354000190377130020</LO><ID>11-0300963</ID></server></inist></record>Pour manipuler ce document sous Unix (Dilib)
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