Analysis of Designer Stimulants by Gc-Ms

ANALYSIS OF DESIGNER
STIMULANTS BY GC/MS
Application Compendium
This page intentionally blank
Table of Contents
Introduction ..........................................................................................................................4
Sample Preparation/Extraction ............................................................................................5
Gas Chromatograph and Mass Spectrometer Conditions ...................................................6
2,5-dimethoxy-4-bromoamphetamine ................................................................................7
2,5-dimethoxy-4-chloroamphetamine .................................................................................8
2,5-dimethoxy-4-ethylphenethylamine ................................................................................9
2,5-dimethoxy-4-ethylthiophenethylamine .......................................................................10
2,5-dimethoxy-4-iodophenethylamine ..............................................................................11
2,5-dimethoxy-4-methylamphetamine ..............................................................................12
2,5-dimethoxy-4-propylthiophenethylamine .....................................................................13
3-trifluoromethylphenylpiperazine .....................................................................................14
3,4-dimethylmethcathinone ...............................................................................................15
3,4-methylenedioxyamphetamine .....................................................................................16
3,4-methylenedioxymethamphetamine .............................................................................17
3,4-methylenedioxymethcathinone ...................................................................................18
4-bromo-2,5-dimethoxyphenethylamine ...........................................................................19
4-fluoromethcathinone ......................................................................................................20
4-methoxymethcathinone ..................................................................................................21
4-methyl-N-ethylcathinone ................................................................................................22
4-methylmethcathinone .....................................................................................................23
5-methoxy-dimethyltryptamine ..........................................................................................24
Benzodioxyolybutanamine .................................................................................................25
Benzylpiperazine ................................................................................................................26
Butylone .............................................................................................................................27
Ethylone ..............................................................................................................................28
Methcathinone ...................................................................................................................29
Methylbenzodioxolylbutanamine .......................................................................................30
Methylenedioxyethylamphetamine ...................................................................................31
Methylenedioxypyrovalerone ............................................................................................32
N,N-diallyl-5-methoxytryptamine ......................................................................................33
Naphyrone .........................................................................................................................34
Pyrovalerone.......................................................................................................................35
Bath Salts GC Analysis .................................................................................................36-38
Analysis of Designer Stimulants

by GC/MS
Application Compendium
Introduction
By Fran Diamond, Chemistry Technical Leader, NMS Labs

A new wave of drugs has swept through the drug community. These new compounds are
chemical variations of older traditional stimulant drugs. Popularly known and labeled as
bath salts, these compounds are synthetic derivatives of psychedelic chemicals known as
cathinones, tryptamines, phenethylamines and piperazines. They are chemically altered so
that they are not technically illegal yet pose the same health risks as the controlled varieties.
These new chemicals vary by slight changes to the chemical structure by placement of alkyl
side-chains, replacement of methyl with ethyl groups, etc. They are packaged and sold under
innocuous names such as Ivory wave ,Vanilla sky, and Tranquility, to name a few, and
under the guise of bath salts or plant food and more recently party powders. These
products are legal. They can be readily purchased at convenience stores, mini-marts, and
headshops. They can also be purchased easily over the internet.
These are dangerous compounds. They have not been tested in humans. Users dont always
know what they are taking or what contaminants are present in these powders. There is no
quality control for these clandestine operations. Users develop hallucinations, paranoia, rapid
heart rates and suicidal thoughts. Despite the sometimes frightening episodes, users tend to
compulsively repeat use. There have been numerous reports of belligerent behavior in users that
require the strength of many people to subdue. These substances have been associated with a
growing number of incidences resulting in violence and fatalities.
Numerous states have enacted legislation banning the use of some of these drugs. The Drug
Enforcement Administration (DEA) recently used its emergency authority to ban chemicals
used in bath salts, calling the chemicals an imminent hazard to the public; but this only
addressed three of the more prevalent chemicals. There are many more of these substances
and even when controlled, newer variations are readily infused. This phenomenon has given
law enforcement and testing laboratories a series of challenges to overcome in order to provide
testing of these new materials. As with the synthetic cannabinoids, which emerged recently,
these newer variations are being manufactured mainly in China and distributed worldwide.
Few legitimate suppliers of reference materials have been able to keep up with numerous
analogous and homologous materials that are used. There are endless possible chemical
variations. To compound the problem, there is abundant information on the internet for
synthesizing these compounds.
Analytical laboratories have had a difficult time obtaining pure reference material to use for
positive identification. As soon as legislation is passed banning their use, different drugs show
up in the next wave. The number of variations is constantly expanding. These materials are also
structurally similar in terms of chromatographic retention time and mass spectral appearance.
There are many isomeric possibilities that require the analysis be capable of measuring slight
variation in data. This can be chromatographic retention or slight differences in mass spectral
fragmentation. Data analysis needs to be able to identify the subtle differences in these species
and be able to find these substances in complex mixtures.
Sample Preparation
Extraction
These compounds are generally basic amine compounds and can be easily extracted into
organic solvent under basic conditions. Since it is not uncommon to find multiple drugs of
various chemical properties, we use an acid/base combined extraction. In this procedure, we
acidify an aliquot of sample (approximately 25 mg of material) by adding 1 mL of de-ionized
water followed by the addition of internal standard and 3 drops of 10% HCl. We next add
1 mL of extraction solvent (95% methylene chloride/5% isopropanol v/v) and mix briefly.
We centrifuge the sample and remove the bottom solvent layer and keep. To the remaining
aqueous mixture, we add 2 drops of concentrated ammonium hydroxide solution and add 1
mL of the above mentioned mixed solvent layer. Tubes are again mixed and centrifuged, and
the lower solvent layer is again removed and combined with the initial solvent. This combined
extract is then mixed briefly and transferred to an autosampler vial and capped. It is now
ready for instrumental analysis.
Gas Chromatograph and Mass Spectrometer Conditions

GC
Agilent technologies 6890 with fast oven, Autoinjector and tray
Inlet
EPC Split/splitless
Mode
Constant pressure
Injection type:
Splitless
Injection volume (uL):
1.0
Inlet temperature (C):
265
Pressure nominal (psig):
21.1
Purge flow (ml/min.):
50
Purge time (min.):
0.30
Gas type:
Helium
Oven
Voltage (VAC):
240
Initial Oven Temp. (C):
50
Initial oven hold (min.):
Ramp rate (C/min.):
30
Final Temp. (C):
340
Final hold (min.):
0.5
Total Run Time (min.):
10.17
Equilibration time (min.):
0.1
Column
Type:
DB-1
Agilent part number:
128-1012
Length (m):
12
Diameter (mm):
0.200
Film Thickness (um):
0.33
Nominal Initial Flow (mL/min):
2.6
MSD
Agilent Technologies 5973 network
Vacuum pump
Turbo
Tune File
Atune.U
Mode
scan
Solvent delay (min.)
1.5
EM voltage
Atune Voltage
Low mass (amu)
40
High mass (amu)
550
Threshold
250
Sampling
Quad temp (C)
150
Source temp (C)
230
Transfer line temp (C)
300
2,5-Dimethoxy-4-bromoamphetamine
Chemical name:
1-(4-Bromo-2,5-dimethoxyphenyl)-2-aminopropane
Abbreviation:
DOB
Molecular formula:
C11H16BrNO2
Molecular mass:
274.15
Major GC/MS ions:
44, 230, 232, 77,105
Ions used for analysis:
Target:
44
Qualifier-1:
230
Qualifier-2:
232
Retention time:
5.21 minutes
LOD:
20 mcg/g
Molecular Structure:
Mass Spectrum:
Abundance
44
750000
700000
650000
600000
550000
500000
450000
400000
350000
300000
250000
200000
150000
230
100000
77
50000
m/z-->
53
40
50
91
63
60
70
80
90
105
100
110
121
120
129 136
130
143149
140
150
157 164 171 179 186192

160
170
180
190
201
200
215
210
220
242
230
240
258
250
260
273
270
280
2,5-Dimethoxy-4-chloroamphetamine
Chemical name:
1-(4-chloro-2,5-dimethoxy-phenyl)propan-2-amine
Abbreviation:
DOC
Molecular formula:
C11H16ClNO2
Molecular mass:
229.70
Major GC/MS ions:
44, 186, 188, 77, 171
Target:
44
Qualifier-1:
186
Qualifier-2:
188
Retention time:
4.90 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
1100000
44
1050000
1000000
950000
900000
850000
800000
750000
700000
650000
600000
550000
500000
450000
400000
350000
300000
186
250000
200000
150000
100000
50000
m/z-->
77
51
57
63
72
85
91
99
105 112
121 127 134 142147
171
155
162
178
198
214
229
35 40 45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200 205 210 215 220 225 230 235
2,5-Dimethoxy-4-ethylphenethylamine
Chemical name:
1-(2,5-Dimethoxy-4-ethylphenyl)-2-aminoethane
Abbreviation:
2C-E
Molecular formula:
C12H19NO2
Molecular mass:
209.29
Major GC/MS ions:
180, 165, 91, 179, 209
Target:
180
Qualifier-1:
165
Qualifier-2:
209
Retention time:
4.64 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
180
750000
700000
650000
600000
550000
500000
450000
165
400000
350000
300000
250000
200000
91
150000
209
77
100000
50000
m/z-->
51
41
35
40
45
50
65
57
55
82
71
60
65
70
75
80
96
85
90
149
117
105
110
134
122
128
144
160
175
190
95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200 205 210 215
2,5-dimethoxy-4-ethylthiophenethylamine
Chemical name:
2-[4-(Ethylthio)-2,5-dimethoxyphenyl]ethanamine
Abbreviation:
2C-T-2
Molecular formula:
C12H19NO2S
Molecular mass:
241.35
Major GC/MS ions:
212, 211, 183, 241, 153
Target:
212
Qualifier-1:
183
Qualifier-2:
241
Retention time:
5.63 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
212
850000
800000
750000
700000
650000
600000
550000
500000
450000
400000
350000
183
300000
241
250000
200000
153
197
150000
100000
50000
m/z-->
45
53 59 65
77
71
91
85
97
103
138
121
109
115
132
167
147
161
177
191
224
234
249
35 40 45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200 205 210 215 220 225 230 235 240 245 250 255
10
2,5-dimethoxy-4-iodophenethylamine
Chemical name:
2,5-dimethoxy-4-iodophenethylamine
Abbreviation:
2C-I
Molecular formula:
C10H14INO2
Molecular mass:
307.13
Major GC/MS ions:
278, 263.0 307, 77, 279
Target:
278
Qualifier-1:
263
Qualifier-2:
307
Retention time:
5.53 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
550000
278
500000
450000
400000
350000
300000
250000
200000
150000
263
100000
77
50000
m/z-->
53
307
91
63
105
43
40
247
121
136
128
50
60
70
80
90
100
110
120
130
140
151
150
164
160
11
170
180
180
191
190
205
200
210
219
220
232
230
291
240
250
260
270
280
290
300
310
2,5-dimethoxy-4-methylamphetamine
Chemical name:
1-(2,5-Dimethoxy-4-methylphenyl)-2-aminopropane
Abbreviation:
DOM, STP
Molecular formula:
C12H19NO2
Molecular mass:
209.29
Major GC/MS ions:
166, 44, 151, 91, 167
Target:
166
Qualifier-1:
44
Qualifier-2:
151
Retention time:
4.45 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
44
850000
166
800000
750000
700000
650000
600000
550000
500000
450000
400000
350000
151
300000
250000
200000
150000
91
77
100000
50000
m/z-->
51
35
40
45
50
135
65
105
55
97
82
57
60
65
70
75
80
85
90
110 117
123
130
146
161
176
194
209
95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200 205 210 215
12
2,5-Dimethoxy-4-propylthiophenethylamine
Chemical name:
2-[2,5-Dimethoxy-4-(propylthio)phenyl]ethanamine
Abbreviation:
2C-T-7
Molecular formula:
C13H21NO2S
Molecular mass:
255.38
Major GC/MS ions:
226, 225, 183, 255, 153
Target:
226
Qualifier-1:
183
Qualifier-2:
255
Retention time:
5.91 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
226
500000
450000
400000
350000
300000
250000
183
200000
150000
255
153
169
100000
50000
41
m/z-->
47
53
59
65
77
71
91
85
97
110
104
138
121
147
132
163
177
195
211
238
35 40 45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200 205 210 215 220 225 230 235 240 245 250 255 260 265
13
3-trifluoromethylphenylpiperazine
Chemical name:
1-[3-(trifluoromethyl)phenyl]piperazine
Abbreviation:
TFMPP
Molecular formula:
C11H13F3N2
Molecular mass:
230.23
Major GC/MS ions:
188, 230, 145, 172, 189
Target:
188
Qualifier-1:
230
Qualifier-2:
145
Retention time:
4.04 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
188
1400000
1300000
1200000
1100000
1000000
900000
800000
700000
600000
500000
400000
230
300000
145
200000
172
56
100000
m/z-->
42
50
63 69
75
83 89
95
125
105 113 119
130
139
152
159
166
180
200
211
35 40 45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200 205 210 215 220 225 230 235 240
14
3,4-dimethylmethcathinone
Chemical name:
1-(3,4-dimethylphenyl)-2-(methylamino)propan-1-one
Abbreviation:
3,4-DMMC
Molecular formula:
C12H17NO
Molecular mass:
191.27
Major GC/MS ions:
58, 77, 79, 105, 133
Target:
58
Qualifier-1:
105
Qualifier-2:
133
Retention time:
4.29 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
58
1200000
1100000
1000000
900000
800000
700000
600000
500000
400000
300000
200000
77
100000
m/z-->
42
46
35
40
45
51
50
63
55
60
65
105
68 73
70
75
81 86
80
85
91
90
98
95
133
113 119
128
139143 148
156 161
176
187191
100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200
15
3,4-methylenedioxyamphetamine
Chemical name:
(R) 1-(benzo[1,3]dioxol-5-yl)propan-2-amine
Abbreviation:
MDA
Molecular formula:
C10H13NO2
Molecular mass:
179.22
Major GC/MS ions:
44, 136, 135, 77, 51
Target:
44
Qualifier-1:
136
Qualifier-2:
77
Retention time:
3.83 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
44
1050000
1000000
950000
900000
850000
800000
750000
700000
650000
600000
550000
500000
136
450000
400000
350000
300000
250000
200000
77
51
150000
100000
50000
m/z-->
63
56
35
40
45
50
55
60
67
65
73
70
75
81
80
105
89 93
85
90
95
131
117 121
100
105
16
110
115
120
125
130
140
145
150
179
164
148
135
155
160
165
170
175
180
185
3,4-methylenedioxymethamphetamine
Chemical name:
(RS)-1-(benzo[d][1,3]dioxol-5-yl)-N-methylpropan-2-amine
Abbreviation:
MDMA
Molecular formula:
C11H15NO2
Molecular mass:
193.25
Major GC/MS ions:
58, 77, 135, 51, 56
Target:
58
Qualifier-1:
135
Qualifier-2:
77
Retention time:
4.08 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
58
1400000
1300000
1200000
1100000
1000000
900000
800000
700000
600000
500000
400000
300000
200000
m/z-->
77
51
100000
42
35
40
63
45
50
55
60
65
135
88
70
70
75
80
85
90
94
95
105
120
148
163
178
192
100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200
17
3,4-methylenedioxymethcathinone
Chemical name:
()-2-methylamino-1-(3,4-methylenedioxyphenyl)propan-1-one
Abbreviation:
Methylone, bk-MDMA
Molecular formula:
C11H13NO3
Molecular mass:
207.23
Major GC/MS ions:
58, 65, 63, 149, 121
Target:
58
Qualifier-1:
121
Qualifier-2:
149
Retention time:
4.76 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
58
1200000
1100000
1000000
900000
800000
700000
600000
500000
400000
300000
200000
65
100000
m/z-->
42
35
40
53
45
50
55
74 79
60
65
70
75
80
95
85
90
149
121
91
135
102
162
176
192
207
95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200 205 210 215
18
4-bromo-2,5-dimethoxyphenethylamine
Chemical name:
2-(4-bromo-2,5-dimethoxyphenyl)ethanamine
Abbreviation:
2C-B
Molecular formula:
C10H14BrNO2
Molecular mass:
260.13
Major GC/MS ions:
230, 232, 215, 217, 77
Target:
230
Qualifier-1:
259
Qualifier-2:
77
Retention time:
5.12 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
230
130000
120000
110000
100000
90000
80000
70000
60000
50000
40000
77
215
30000
20000
105
91
53
63
10000
43
m/z-->
69
85
98
115
261
201
121
129
136
143
150
157 164
171
180
186
207
221
242
249
35 40 45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200 205 210 215 220 225 230 235 240 245 250 255 260 265 270
19
4-fluoromethcathinone
Chemical name:
(RS)-1-(4-fluorophenyl)-2-methylaminopropan-1-one
Abbreviation:
Flephedrone, 4-FMC
Molecular formula:
C10H12FNO
Molecular mass:
181.206
Major GC/MS ions:
58, 95, 75, 56, 123
Target:
58
Qualifier-1:
95
Qualifier-2:
123
Retention time:
3.12 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
1200000
58
1100000
1000000
900000
800000
700000
600000
500000
400000
300000
95
200000
75
123
42
100000
50
m/z-->
35
40
45
50
63
54
55
60
65
69
70
103 109
83 87
75
80
85
90
95
100
105
20
110
151
133 138
115
120
125
130
135
140
145
150
166
155
160
165
180
170
175
180
185
4-Methoxymethcathinone
Chemical name:
RS)-1-(4-methoxyphenyl)-2-(methylamino)propan-1-one
Abbreviation:
Methedrone
Molecular formula:
C11H15NO2
Molecular mass:
193.242
Major GC/MS ions:
58, 77, 92, 135, 64
Target:
58
Qualifier-1:
92
Qualifier-2:
135
Retention time:
4.43 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
1200000
58
1100000
1000000
900000
800000
700000
600000
500000
400000
300000
200000
77
100000
m/z-->
35
40
92
64
42
135
107
50
45
50
55
60
65
70
75
80
85
90
95
117121
150
163
178
193
100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200
21
4-methyl-N-ethylcathinone
Chemical name:
(RS)-2-ethylamino-1-(4-methylphenyl)propan-1-one
Abbreviation:
4-MEC
Molecular formula:
C12H17NO
Molecular mass:
191.27
Major GC/MS ions:
72, 44, 91, 65, 119
Target:
72
Qualifier-1:
44
Qualifier-2:
119
Retention time:
4.01 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
1600000
72
1500000
1400000
1300000
1200000
1100000
1000000
900000
800000
700000
600000
500000
44
400000
300000
200000
100000
m/z-->
91
65
51
35
40
45
50
119
56
55
77
60
65
70
75
105
86
80
85
90
95
128 133
146
160
176
191
100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195
22
4-methylmethcathinone
Chemical name:
(RS)-2-methylamino-1-(4-methylphenyl)propan-1-one
Abbreviation:
Mephedrone, 4-MMC
Molecular formula:
C11H15NO
Molecular mass:
177.242
Major GC/MS ions:
58, 91, 65, 56, 42
Target:
58
Qualifier-1:
91
Qualifier-2:
42
Retention time:
3.74 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
58
1400000
1300000
1200000
1100000
1000000
900000
800000
700000
600000
500000
400000
300000
200000
100000
m/z-->
91
65
42
35
40
119
51
45
50
77
55
60
65
70
75
105
87
80
85
90
95
100
105
23
115
110
115
125
130
135
162
147
133
120
140
145
150
155
160
165
177
170
175
180
185
5-methoxy-dimethyltryptamine
Chemical name:
2-(5-methoxy-1H-indol-3-yl)-N,N-dimethylethanamine
Abbreviation:
5-MeO-DMT
Molecular formula:
C13H18N2O
Molecular mass:
218.298
Major GC/MS ions:
58, 218, 160, 117, 145
Target:
58
Qualifier-1:
160
Qualifier-2:
218
Retention time:
5.88 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
58
1500000
1400000
1300000
1200000
1100000
1000000
900000
800000
700000
600000
500000
400000
300000
200000
m/z-->
117
42
100000
35
40
45
50
55
60
65
89
77
63
51
70
75
80
85
90
130
103
140
218
160
145
155
174
187
201
95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200 205 210 215 220 225
24
Benzodioxyolybutanamine
Chemical name:
1-(1,3-benzodioxol-5-yl)butan-2-amine
Abbreviation:
BDB
Molecular formula:
C11H15NO2
Molecular mass:
193.242
Major GC/MS ions:
58, 136, 135, 77, 41
Target:
58
Qualifier-1:
136
Qualifier-2:
77
Retention time:
4.29 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
58
950000
900000
850000
800000
750000
700000
650000
600000
550000
500000
450000
400000
350000
300000
136
250000
200000
77
150000
41
100000
51
50000
m/z-->
63
35
40
45
50
55
60
65
81
106
89 94
70
70
75
80
85
90
95
164
115 121
131
147
176
193
100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200
25
Benzylpiperazine
Chemical name:
1-benzylpiperazine
Abbreviation:
BZP
Molecular formula:
C11H16N2
Molecular mass:
176.258
Major GC/MS ions:
91, 134, 56, 176, 65
Target:
91
Qualifier-1:
134
Qualifier-2:
176
Retention time:
3.90 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
91
850000
800000
750000
700000
650000
600000
134
550000
500000
450000
400000
350000
300000
250000
56
200000
100000
85
42
50000
m/z-->
176
65
150000
51
71
61
35
40
45
50
55
60
65
70
77
75
120
99
81
80
85
90
95
100
104
105
26
146
130
116
110
115
120
125
130
159
135
140
145
150
155
160
165
170
175
180
185
Butylone
Chemical name:
1-(1,3-benzodioxol-5-yl)-2-(methylamino)butan-1-one
Abbreviation:
bk-MBDB
Molecular formula:
C12H15NO3
Molecular mass:
221.2524
Major GC/MS ions:
72, 65, 63, 57, 121
Target:
72
Qualifier-1:
121
Qualifier-2:
57
Retention time:
5.05 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
72
1200000
1100000
1000000
900000
800000
700000
600000
500000
400000
300000
200000
100000
m/z-->
65
57
44
51
35
40
45
50
77
55
149
121
60
65
70
75
84
80
85
91
90
96
105
130 135
116
144
162
172 177
187 192
204
214 221
95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200 205 210 215 220 225 230
27
Ethylone
Chemical name:
(RS)-1-(1,3-benzodioxol-5-yl)-2-(ethylamino)propan-1-one
Abbreviation:
bk-MDEA
Molecular formula:
C12H15NO3
Molecular mass:
221.2524
Major GC/MS ions:
72, 44, 65, 63, 149
Target:
72
Qualifier-1:
44
Qualifier-2:
149
Retention time:
4.99 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
72
1100000
1000000
900000
800000
700000
600000
500000
400000
44
300000
200000
65
100000
m/z-->
51
35
40
45
50
55
77
60
65
70
75
135
103
80
85
90
149
121
91
56
162
178
190
206
220
95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200 205 210 215 220 225
28
Methcathinone
Chemical name:
((RS)-2-(methylamino)-1-phenyl-propan-1-one
Abbreviation:
Molecular formula:
C10H13NO
Molecular mass:
163.22
Major GC/MS ions:
58, 77, 51, 56, 42
Target:
58
Qualifier-1:
77
Qualifier-2:
105
Retention time:
3.19 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
1200000
58
1100000
1000000
900000
800000
700000
600000
500000
400000
300000
77
200000
51
100000
m/z-->
42
63
35
40
45
50
55
60
86
73
65
70
75
80
85
105
91
90
29
100
105
110
115
120
148
133
115 120
95
125
130
135
140
145
150
162
155
160
165
170
Methylbenzodioxolylbutanamine
Chemical name:
(RS)-1-(1,3-Benzodioxol-5-yl)-N-methylbutan-2-amine
Abbreviation:
MBDB
Molecular formula:
C12H17NO2
Molecular mass:
207.27
Major GC/MS ions:
72, 135, 77, 57, 51
Target:
72
Qualifier-1:
135
Qualifier-2:
57
Retention time:
4.47 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
72
1700000
1600000
1500000
1400000
1300000
1200000
1100000
1000000
900000
800000
700000
600000
500000
400000
300000
200000
m/z-->
51
42
100000
135
77
57
88
63
35
40
45
50
55
60
65
93
70
75
80
85
90
105
115 120
130
148
178
163
206
95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200 205 210 215
30
Methylenedioxyethylamphetamine
Chemical name:
1-(1,3-benzodioxol-5-yl)-N-ethyl-propan-2-amine
Abbreviation:
MDEA
Molecular formula:
C12H17NO2
Molecular mass:
207.27
Major GC/MS ions:
72, 44, 135, 77, 51
Target:
72
Qualifier-1:
135
Qualifier-2:
44
Retention time:
4.29 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
72
1700000
1600000
1500000
1400000
1300000
1200000
1100000
1000000
900000
800000
700000
600000
500000
400000
44
300000
51
100000
m/z-->
135
77
200000
56
35
40
45
50
55
63
60
65
91 96
81
70
75
80
85
90
105
115 121
147
163
176
192
206
95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200 205 210 215
31
Methylenedioxypyrovalerone
Chemical name:
(RS)-1-(Benzo[d][1,3]dioxol-5-yl)-2-(pyrrolidin-1-yl)pentan-1-one
Abbreviation:
MDPV
Molecular formula:
C16H21NO3
Molecular mass:
275.343
Major GC/MS ions:
126, 127, 65, 149, 55
Target:
126
Qualifier-1:
65
Qualifier-2:
149
Retention time:
6.34 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
126
1600000
1500000
1400000
1300000
1200000
1100000
1000000
900000
800000
700000
600000
500000
400000
300000
200000
100000
m/z-->
42
65
55
77
40
50
60
70
80
84
96
90
149
103 110 119
100
110
120
135
130
140
177
164
150
32
160
170
180
190
190
204
200
216
210
220
232
230
246
240
250
273
260
270
280
N,N-diallyl-5-methoxytryptamine
Chemical name:
N-allyl-N-[2-(5-methoxy-1H-indol-3-yl)ethyl]prop-2-en-1-amine
Abbreviation:
5-MeO-Dalt
Molecular formula:
C17H22N2O
Molecular mass:
270.375
Major GC/MS ions:
110, 41, 160, 111, 117
Target:
110
Qualifier-1:
160
Qualifier-2:
41
Retention time:
6.81 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
110
1700000
1600000
1500000
1400000
1300000
1200000
1100000
1000000
900000
800000
700000
600000
500000
400000
41
300000
160
200000
117
100000
m/z-->
55
40
50
81
68
75
62
60
70
80
90
90
130
96 103
100
145
174
154
110
120
130
140
150
33
160
170
186
180
190
199
200
229
214
210
220
230
270
241
240
250
260
270
Naphyrone
Chemical name:
1-naphthalen-2-yl-2-pyrrolidin-1-ylpentan-1-one
Abbreviation:
NRG-1
Molecular formula:
C19H23NO
Molecular mass:
281.391
Major GC/MS ions:
126, 127, 55, 42, 96
Target:
126
Qualifier-1:
127
Qualifier-2:
55
Retention time:
6.92 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
126
3800000
3600000
3400000
3200000
3000000
2800000
2600000
2400000
2200000
2000000
1800000
1600000
1400000
1200000
1000000
800000
600000
400000
200000
m/z-->
55
42
40
62
50
60
69
70
96
77 84
80
90
100
110
110
141
120
130
140
155
150
34
165
160
170
181
180
195
190
200
210
220
210
220
238
230
240
280
250
250
260
270
280
Pyrovalerone
Chemical name:
(RS)-1-(4-methylphenyl)-2-(1-pyrrolidinyl)pentan-1-one
Abbreviation:
Molecular formula:
C16H23NO
Molecular mass:
245.36
Major GC/MS ions:
126, 127, 91, 65, 55
Target:
126
Qualifier-1:
91
Qualifier-2:
65
Retention time:
5.49 minutes
LOD:
20 mcg/g
Mass Spectrum:
Abundance
126
3400000
3200000
3000000
2800000
2600000
2400000
2200000
2000000
1800000
1600000
1400000
1200000
1000000
800000
600000
400000
200000
m/z-->
42
55
91
65
71 77
84
97
103 110
119
132
141 147
159
174
186
202
216
244
35 40 45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200 205 210 215 220 225 230 235 240 245 250
35
Bath Salts Analysis

Introduction
Spectra obtained for all bath salts on the Agilent 240 Ion Trap GC/MS are comparable to
spectra generated on the Agilent 5973 GC/MSD. The bath salts Designer Drugs Library created
using spectra from the Agilent 5973 GC/MSD were used to accurately identify all analytes of
interest in this study. Chromatograms and spectra obtained on the Agilent Technologies 240 Ion
Trap GC/MS were seamlessly interpreted using Agilents MassHunter Workstation Software
for qualitative and quantitative analysis. LOD for most analytes of interest was 1ppb in Full
Scan mode. Whether you want to analyze bath salts by Quadruple or Ion Trap GC/MS, Agilent
Technologies has the solution to your laboratorys cutting-edge and complex forensic problems.
36
Bath Salts Analysis
Full Scan Total Ion Chromatogram of Bath Salts Mixture (100ppb in MeoH) on the Agilent 240 Ion Trap GC/MS
Bath Salt Analyte
1: 4-Fluoromethcathinone
2: Methcathinone
3: 3,4-Dimethylmethcathinone
4: 4-Methylmethcathinone
5: Methylenedioxyamphetamine (MDA)
6: Benzylpiperazine (BZP)
7: 4-Methyl-N-ethylcathinone
8: 3-Trifluoromethylphenylpiperazine (TFMPP)
9: Methylenedioxymethamphetamine (MDMA)
10: Methylenedioxyethylamphetamine (MDEA)
11: Benzodioxolylbutanamine
12: 2,5-Dimethoxy-4-methylamphetamine
13: 4-Methoxymethcathinone
14: Methylbenzodioxolylbutanamine
15: 2,5-Dimethoxy-4-ethylphenethylamine
R.T. (min)
6.935
7.135
8.272
8.804
9.208
9.418
9.671
9.899
10.03
10.776
10.934
11.331
11.521
11.531
12.132
Bath Salt Analyte

16: 3,4-methylenedioxymethcathinone
17: 2,5-Dimethoxy-4-chloroamphetamine
18: Ethylone
19: Butylone
20: 4-Bromo-2,5-dimethoxyphenethylamine
21: 2,5-Dimethoxy-4-bromoamphetamine
22: Methylenedioxypyrovalerone (MDPV)
23: 2,5-Dimethoxy-4-iodophenethylamine
24: 2,5-Dimethoxy-4-ethylthiophenethylamine
25: 2,5-Dimethoxy-4-propylthiophenethylamine
26: 5-Methoxy-dimethyltryptamine
27: Methylenedioxypyrovalerone (MDPV)
28: Benzylpiperazine (BZP)
29: N,N-diallyl-5-methoxytryptamine
30: Naphyrone
37
R.T. (min)
13.064
13.412
13.986
14.198
14.647
14.773
15.715
16.081
16.383
17.35
17.416
18.76
19.033
20.278
20.513
Bath Salts Analysis

Baths Salts Anlysis: Agilent 240 Ion Trap MS Conditions:

Scan type: Full Scan

Ionization: EI

Scan Mode: Fast

uScan Averaged: 1uScans

Count Threshold: 1

Target TIC: 40000 Counts

Emission Current: 10uAmps

Mass Range: 43 350 m/z

Tune Type: Auto

Solvent Delay: 3 min

Trap Temperature: 200 C
Manifold Temperature: 100 C
Bath Salts Analysis: Agilent 7890A GC Conditions:

Column: Agilent J&W Factor Four VF-5ms 30m x 0.250mm x 0.25um (p/n: CP8944)

Carrier gas: Helium, 1.2mL/min, Constant Flow

Oven: Temperature Programmed
Inlet: Multi Mode Inlet, 1.0uL injection volume
Inlet Liner: 2 mm Dimpled Deactivated Liner (Part No 5190-2296)

MS Transfer Line: 300 C
38
This page intentionally blank
39
This information is subject to change without notice.

Agilent Technologies, Inc. 2012
Published in USA, December 3, 2012
5990-0001EN

Analysis of Designer Stimulants by Gc-Ms

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Analysis of Designer Stimulants by Gc-Ms

Uploaded by

Copyright:

Available Formats

ANALYSIS OF DESIGNER

This page intentionally blank

Analysis of Designer Stimulants

By Fran Diamond, Chemistry Technical Leader, NMS Labs

Gas Chromatograph and Mass Spectrometer Conditions

Injection volume (uL):

Inlet temperature (C):

Pressure nominal (psig):

Purge flow (ml/min.):

Purge time (min.):

Initial Oven Temp. (C):

Initial oven hold (min.):

Ramp rate (C/min.):

Final Temp. (C):

Final hold (min.):

Total Run Time (min.):

Equilibration time (min.):

Agilent part number:

Film Thickness (um):

Nominal Initial Flow (mL/min):

Solvent delay (min.)

Low mass (amu)

High mass (amu)

Quad temp (C)

Source temp (C)

Transfer line temp (C)

Major GC/MS ions:

44, 230, 232, 77,105

Ions used for analysis:

157 164 171 179 186192

Major GC/MS ions:

44, 186, 188, 77, 171

Ions used for analysis:

121 127 134 142147

Major GC/MS ions:

180, 165, 91, 179, 209

Ions used for analysis:

Major GC/MS ions:

212, 211, 183, 241, 153

Ions used for analysis:

Major GC/MS ions:

278, 263.0 307, 77, 279

Ions used for analysis:

Major GC/MS ions:

166, 44, 151, 91, 167

Ions used for analysis:

Major GC/MS ions:

226, 225, 183, 255, 153

Ions used for analysis:

Major GC/MS ions:

188, 230, 145, 172, 189

Ions used for analysis:

Major GC/MS ions:

58, 77, 79, 105, 133

Ions used for analysis:

Major GC/MS ions:

44, 136, 135, 77, 51

Ions used for analysis:

Major GC/MS ions:

58, 77, 135, 51, 56

Ions used for analysis:

Major GC/MS ions:

58, 65, 63, 149, 121