Application Note # MS-14 - Bruker · Analytical conditions E²M with mounted GC in injector mode:...
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Bruker Daltonics For the detection of drugs a couple of quick tests are avail- able which were used by the police departments and the State Offices of Criminal Investigations. These tests are limited to substance specific reactions and do not give any information about different drug compositions (thin down compounds, by-products, precursors, impurities etc.) which were necessary for criminal investigations. For a clear identification of complex mixtures GC/MS is still the method of choice. With the mobile GC/MS system E²M a fast and inexpensive detection and identification of drugs can be accomplished directly at the scene of crime. This application note demonstrates the time saving determination of differ- ent drugs/drug compositions with the E²M in the GC mode and by direct measurements with the Air/Surface probe. Sampling preparation For this application note the following solutions were pre- pared by dissolving the raw material in methanol (hashish: 4.7 mg/ml, marihuana: 2.2 mg/ml, morphine: 2.8 mg/ml, cocaine: 2.2 mg/ml, heroin: 2.6 mg/ml). For the identifica- tion on-site (not quantification) where a microbalance may not be present this can be done by transferring the amount of one micro-spatula tip (1 – 5 mg) into a vial filled with 1 ml methanol. Application Note # MS-14 Fast On-site Identification of Drugs with the mobile GC/MS system E²M Figure 1: Opium poppy yields the raw material for morphine and heroin production..
Transcript of Application Note # MS-14 - Bruker · Analytical conditions E²M with mounted GC in injector mode:...
Bruker Daltonics
For the detection of drugs a couple of quick tests are avail-able which were used by the police departments and the State Offices of Criminal Investigations. These tests are limited to substance specific reactions and do not give any information about different drug compositions (thin down compounds, by-products, precursors, impurities etc.) which were necessary for criminal investigations. For a clear identification of complex mixtures GC/MS is still the method of choice. With the mobile GC/MS system E²M a fast and inexpensive detection and identification of drugs can be accomplished directly at the scene of crime. This application note demonstrates the time saving determination of differ-ent drugs/drug compositions with the E²M in the GC mode and by direct measurements with the Air/Surface probe.
Sampling preparation
For this application note the following solutions were pre-pared by dissolving the raw material in methanol (hashish: 4.7 mg/ml, marihuana: 2.2 mg/ml, morphine: 2.8 mg/ml, cocaine: 2.2 mg/ml, heroin: 2.6 mg/ml). For the identifica-tion on-site (not quantification) where a microbalance may not be present this can be done by transferring the amount of one micro-spatula tip (1 – 5 mg) into a vial filled with 1 ml methanol.
Application Note # MS-14
Fast On-site Identification of Drugs with the mobile GC/MS system E²M
Figure 1: Opium poppy yields the raw material for morphine and heroin production..
Analytical conditions
E²M with mounted GC in injector mode: 3.5 m HP5-ms, 0.32 mm ID, 1 µm film. injector temperature: 240°, hold-time: 10s, charg-ing time: 30s, pressure during charging: 600 mbar, GC temperature program: 100° to 240° at 15°/min (hold: 600s), carrier gas: ambient air at 1.5 ml/min, MS Scan: 46 – 350 u, integration time: 5 ms/mass; injected volume: 1µl.
E²M with mounted Air/Surface probe: probe head temperature: 240°, probe line tempera-ture: 220°, sampling pump pressure; 850 mbar. MS Scan: 46 – 350 u, integration time: 5ms/mass; sampling: 1µl with probe (press-ing probe head on the sample).
Chromatogram and appropriate mass spectra from a morphine sample
Figure 2: GC run; Injection: 1µl morphine solution (2.8 mg/ml): Beside morphine the derivate ethyl morphine was identified.
5 9 .0 8 1 .09 4 .0
1 2 4 .0
1 4 6 .0
1 6 2 .0
2 1 4 .0 2 5 6 .02 8 4.0
3 1 3 .01 . +M S , D isse ct , 48 3 .6 -5 0 8 .0 s # (1 7 7 -1 8 6 )
2 9 .0
4 2 .05 9 .0
8 1 .09 4 .0
1 2 4 .0
1 4 6 .0
1 6 2 .0
1 7 5 .02 1 4 .0 2 4 3 .0 2 8 4.0
3 1 3 .0
OH
O
N
O
1 . N ist : E th yl m o rp h in e ; Q E I +M S (P : 7 9 2 , F: 8 6 1 , R : 8 9 3 , M : 1 0 0 0 )
7 0 .09 4 .0
1 2 4 .01 6 2 .0 2 1 5.0
2 6 8 .0
2 8 5 .0
3 1 3 .0
2 . +M S , D isse ct , 47 8 .2 -5 1 3 .4 s # (1 7 5 -1 8 8 )
1 7 .03 1.0
4 2 .05 9 .0
9 4 .01 2 4 .0
1 6 2 .0
17 4 .02 1 5.0
2 8 5 .0
O
HO
HO
N
2 . N ist : M o rp h in e ; Q E I +M S (P : 7 9 0 , F: 8 2 8 , R : 9 2 6 , M : 1 0 0 0 )
0 .0
0 .5
1 .0
1 .5
2 .0
2 .5
5x1 0
In te n s.
0
2 5 0
5 0 0
7 5 0
1 0 0 0
1 2 5 0
0 .0
0 .5
1 .0
1 .5
2 .0
2 .5
5x1 0
0
2 5 0
5 0 0
7 5 0
1 0 0 0
1 2 5 0
5 0 1 0 0 1 5 0 2 0 0 2 5 0 3 0 0 3 5 0 m /z
12
2 0 0 4 0 0 6 0 0 8 0 0 1 0 0 0 1 2 0 0 T i m e [s]0
1
2
3
6x1 0
In te n s.
# RT [s] Area Compound Name Library CAS# Purity'
1 490.4 17050945 Ethylmorphine Nist 76-58-4 792
2 493.5 17312711 Morphine Nist 57-27-2 790
Identified substances morphine sample
Chromatogram and appropriate mass spectra from a cocaine sample
Chromatogram and appropriate mass spectra from a hashish sample
Figure 4: GC run; Injection: 1µl hashish solution (4.7 mg/ml): two typical components of hashish / marihuana identified: Cannabinol, THC; Analytical conditions: see E²M with mounted GC in injector mode.
1
2 0 0 40 0 60 0 8 00 10 0 0 12 0 0 Tim e [s]
1
2
3
4
5
6
6x1 0
In te ns.
5 1.0
8 2 .0
10 5 .0
1 2 2.0
1 5 5.0
1 82 .0
2 7 2.030 3 .0
1 . + MS, 8 6 .6 -23 4 .4s # (4 2 -11 2 )
4 2 .0
68 .0
8 2 .0
1 2 2.0 15 2 .0
1 82 .0
19 8 .0 2 7 2.030 3 .0
5 1.0
8 2 .0
10 5 .0
1 2 2.0
1 5 5.0
1 82 .0
2 7 2.030 3 .0
1 . + MS, 8 6 .6 -23 4 .4s # (4 2 -11 2 )
4 2 .0
68 .0
8 2 .0
1 2 2.0 15 2 .0
1 82 .0
19 8 .0 2 7 2.030 3 .0
55 .0 69 .0 91 .0 1 21 .0 1 74 .0 19 3 .0
2 31 .0
2 43 .0
27 1 .0
29 9 .0
314 .01 . + M S , D i sse ct, 48 9 .1 -51 8 .8s # (1 79 -1 90 )
41 .0
55 .0 69 .081 .091 .0 1 07 .0 1 74 .0 19 3 .0
2 31 .0
2 43 .0
27 1 .0
314 .0
O
OH
1 . Ni st : 6 H-Di b enzo [b ,D]p yra n -1 -o l , 6 a ,7 ,8 ,1 0a -te t rah yd ro -6 ,6 ,9 -t rim e th y l-3 -p en ty l -; Q E I +M S (P : 84 7 , F: 903 , R: 91 2 , M : 10 00 )
238 .0
29 5 .0
3 10 .0
2 . + M S , D i sse ct, 49 9 .9 -52 6 .9s # (1 83 -1 93 )
4 3 .0 16 5 .0 22 3 .0
238 .0
2 51 .0
29 5 .0
3 10 .0
OH
O
2 . Ni st : Ca nna b i no l ; Q E I +M S (P : 93 9 , F: 945 , R: 98 0 , M : 10 00 )
0 .0
0 .5
1 .0
1 .5
5x1 0
In tens.
0
25 0
50 0
75 0
100 0
125 0
0
2
4
6
5x1 0
0
25 0
50 0
75 0
100 0
125 0
50 100 15 0 20 0 25 0 3 00 3 50 m /z
Figure 3: Direct sampling of 1µl cocaine solution (2.2 mg/ml) from a surface with E²M Air/Sur-face probe; Analytical conditions: see E²M with mounted Air/Surface probe.
# RT [s] Area Compound Name Library CAS# Purity'
1 119.8 304612217 Cocaine Nist 50-36-2 847
Identified substances cocaine sample
1
2
1 0 0 20 0 3 0 0 4 0 0 50 0 6 00 7 0 0 80 0 9 0 0 1 0 00 T im e [s]0 .0
0 .5
1 .0
1 .5
2 .0
2 .5
6x1 0
In ten s.
Chromatogram and appropriate mass spectra from a heroin sample
Figure 6: GC run; Injection: 1µl heroin solution (2.6 mg/ml): Beside diacetylmorphine (heroin) the compounds acetylcodein and novocaine were identified which are typical thin down compounds of heroin; Analytical conditions: see E²M with mounted GC in injector mode.
5 9 .0 8 1 .09 4 .0 1 2 4 .0 1 6 2 .0
2 0 4 .0 2 6 8 .0 31 0 .0
3 2 7 .03 6 9 .0
3 . +M S , D isse ct , 5 1 1 .0 -5 5 1 .6 s # (1 8 7 -2 0 2 )
1 5 .0
4 3 .0
8 1 .09 4 .0 1 2 4 .0 1 4 6 .0
2 0 4 .0
2 6 8 .0 31 0 .0
3 2 7 .0
3 6 9 .0
O OO
N
O
O3 . N i st : Di a ce tylm o rp h i n e ; Q E I +M S (P : 8 8 2 , F: 9 5 4 , R : 9 1 3 , M : 1 0 0 0 )
0 .0
0 .2
0 .4
0 .6
0 .8
5x1 0
In te n s.
0
2 5 0
5 0 0
7 5 0
1 0 0 0
1 2 5 0
5 0 1 0 0 1 5 0 2 0 0 2 5 0 3 0 0 3 5 0 m /z
1
2
3
2 0 0 4 0 0 6 0 0 8 0 0 1 0 0 0 1 2 00 1 40 0 T i m e [s]0
2
4
6
8
6x1 0
Inte n s.
T IC + D isse ct: , Cm p d 1 , 4 2 8 .1 s D isse ct: , Cm p d 2 , 5 0 2 .5 s
Di sse ct :, Cm p d 3 , 5 26 .5 s
# RT [s] Area Compound Name Library CAS# Purity'
1 495.5 11662059Tetrahydrocannabinol (THC)
Nist 33086-25-8 847
2 505.8 15867883 Cannabinol Nist 521-35-7 939
Identified substances hashish sample
# RT [s] Area Compound Name Library CAS# Purity'
1 428.1 55787740 Novocaine Nist 59-46-1 941
2 502.5 1991596 Acetylcodein Nist 716
3 526.5 8490099 Diacetylmorphine (Heroin) Nist 561-27-3 882
Identified substances heroin sample
Figure 5: Asian heroin.
Chromatogram and appropriate mass spectra from an unknown sample
63 .0
92 .0
1 2 0 .0
1 38 .0
18 0 .0
2 . + M S , Di sse ct, 8 6 .2-1 1 0 .5 s #(3 0 -39 )
43 .0
6 4 .0
92 .0
1 2 0 .0
1 38 .0
18 0 .0
O OH
O O
2 . N ist: A sp i ri n ; Q E I + M S (P : 9 5 3, F : 96 3 , R: 96 0 , M : 1 0 00 )0
1
2
3
4
5
5x 10
In te ns.
0
2 5 0
5 0 0
7 5 0
10 0 0
12 5 0
5 0 1 0 0 1 5 0 2 00 25 0 3 0 0 3 5 0 m /z
1
2
3
10 0 2 00 3 0 0 40 0 5 0 0 6 0 0 70 0 8 0 0 T i m e [s]0
1
2
3
4
6x10
In te n s.
Figure 8: GC run; Injection: 1µl unknown solution (2.2 mg/ml): Results show that no drug is present; sample is just rotten Aspirin® (Aspirin + salicylic acid) with some caffeine; Analytical conditions: see E²M with mounted GC in injector mode.
Figure 7: Unknown sample confiscated by the police and suspected of being a drug.
# RT [s] Area Compound Name Library CAS# Purity'
1 55.6 27522076 Salicylic Acid Nist 69-72-7 956
2 95.5 12232044 Aspirin Nist 50-78-2 953
3 150.8 1072028 Caffeine Nist 58-08-2 710
Identified substances unknown sample
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© B
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MS
-14
Bruker Daltonik GmbH
Bremen · GermanyPhone +49 (421) 2205-0 Fax +49 (421) 2205-103 [email protected]
Bruker Daltonics Inc.
Billerica, MA · USAPhone +1 (978) 663-3660 Fax +1 (978) 667-5993 [email protected]
www.brukerdetection.com
Author
Dr. Thomas Ludwig, Application CBRNE, Bruker Daltonik GmbH, [email protected]
Keywords:
Onsite Analysis
Mobile GC/MS
Fast drug detection
Instrumentation & Software
Mobile GC/MS System E²M
E²M Software Package
For research use only. Not for use in diagnostic procedures.
Figure 9: Mobile GC/MS system E²M
Conclusions
With the mobile GC/MS system E²M drugs (here: hashish, marihuana, morphine, cocaine, heroin) can be identified directly on the scene of crime within 10 – 15 min. The operation of the system is reduced to the lowest possible level so that non-chemists are able to run the system. In comparison to classical investigations (laboratory measurements), which are time consuming, and expensive identification of drugs can be carried out quickly and at low cost. Therefore the GC/MS system E²M is a powerful analytical tool to save time and money.
