Upload
others
View
3
Download
0
Embed Size (px)
Citation preview
Test report Number 8866 5
Object of analysis: 8866 5
Customer: Samples: 1
Batch: Arrived on: 2020/02/22
Subject: Identification, other ingredients, density measurement, quantification
Method(s): NMR (nuclear magnetic resonance spectroscopy) qNMR (quantitative NMR)
Instrumentation: Bruker Avance III 700 MHz NMR spectrometer Mettler Toledo ME204 analytical balance Hamilton 1 mL gastight syringe, model 1001 TLL
Sample / Analysis Method Status Result Value
8866 5:
Identification NMR N Testosterone enanthate [315-37-7] Identified
Other ingredients NMR N Benzyl benzoate [120-51-4] Benzyl alcohol [100-51-6] Ricinolein [2540-54-7] Ethyl oleate [111-62-6]
Identified
Density Mass divided by
volume
N ρoil=
0.8562 g 0.83 mL
= 1.03 g
mL 1.03
gmL
Quantification qNMR N Component
Testosterone enanthate Benzyl benzoate Benzyl alcohol Ricinolein Ethyl oleate
Mass%
30.8% 10.8% 1.9%
28.9% 26.0%
mg/mL
318 mg/mL 112 mg/mL 19 mg/mL
298 mg/mL 268 mg/mL
Method status: G = GMP A = accreditated V = generally validated P = validated on product N = not validated E = external lab
Remarks: “8866 5” contained testosterone enanthate.
The uncertainty of volume measurement using Hamilton 1 mL syringe was ±0.01 mL.
Signatures: Date: 2020/03/03
Quantitative analysis of the "8866 5" sample
For the ¹H qNMR experiment, 64 scans were acquired, recycling delay was set to 20 seconds, 90° pulse was used.
Compound [CAS number] Molar mass Weight taken
Chemical shift
of chosen ¹H
NMR signal
Integral of that
¹H NMR signal
Number of H's
under that
signal
Content in
the oil
(mass%)
Sum mg/mL
Testosterone enanthate [315-37-7] 400.59 g/mol 5.62 ppm 1.0000 1 30.8% 318 mg/mL
Benzyl benzoate [120-51-4] 212.25 g/mol 8.05 ppm 1.3254 2 10.8% 112 mg/mL
Benzyl alcohol [100-51-6] 108.14 g/mol 7.21 ppm 0.2230 1 1.9% 19 mg/mL
Ricinolein [2540-54-7] 933.45 g/mol 4.17 ppm 0.8045 2 28.9% 298 mg/mL
Ethyl oleate [111-62-6] 310.52 g/mol 4.06 ppm 2.1742 2 26.0% 268 mg/mL
1,4-Dimethoxybenzene [150-78-7] 138.17 g/mol 0.0725 g 6.82 ppm 20.0764 4 99.0%
Reference for the calculation method:
https://doi.org/10.1016/j.jpba.2010.02.007
0.1345 g of the oil ("8866 5") and 0.0725 g of 1,4-dimethoxybenzene (99+% purity) were directly weighed into an NMR tube, and 0.6 mL of acetone-d6 was added.
Shaked at room temperature, giving a homogeneous solution.
Rundlöf, T.; Mathiasson, M.; Bekiroglu, S.; Hakkarainen, B.; Bowden, T.; Arvidsson, T. Survey and qualification of internal standards for quantification by ¹H NMR
spectroscopy, J. Pharm. Biomed. Anal. 2010, 52, 5, 645-651.
0.1345 g 98.4%
* In this sample the carrier oil was ethyl oleate and ricinolein.
https://en.wikipedia.org/wiki/Ethyl_oleate
https://en.wikipedia.org/wiki/Ricinolein
� Photo of the sample
8866 5
10.0 9.5 9.0 8.5 8.0 7.5 7.0 6.5 6.0 5.5 5.0 4.5 4.0 3.5 3.0 2.5 2.0 1.5 1.0 0.5 0.0 ppm
-0.000
0.842
0.873
0.880
0.883
1.177
1.183
1.193
1.203
1.285
1.302
1.309
1.460
1.465
1.472
1.475
1.481
1.487
1.490
1.536
1.541
1.556
1.566
1.577
1.588
1.599
1.605
1.621
1.626
1.640
1.738
1.756
1.974
1.976
2.019
2.021
2.024
2.028
2.038
2.048
2.060
2.069
2.170
2.189
2.199
2.207
2.216
2.231
2.238
2.249
2.259
2.265
2.271
2.276
2.281
2.287
2.290
2.297
2.301
2.307
2.312
2.317
2.350
2.357
2.374
3.702
4.046
4.057
4.067
4.077
4.171
4.180
4.188
4.319
4.324
4.579
4.591
4.603
4.627
5.341
5.349
5.358
5.446
5.473
5.618
6.822
7.327
7.370
7.381
7.392
7.467
7.475
7.477
7.477
7.485
7.486
7.488
7.599
8.044
8.046
8.056
8.057
3.1
195
10.7
422
1.0
430
0.9
291
7.4
072
49.6
052
3.3
092
10.3
516
0.9
496
0.9
452
1.2
267
7.5
365
1.1
941
10.7
480
1.9
951
0.2
380
0.5
435
1.1
810
30.3
583
2.1
742
0.8
045
0.7
686
1.0
229
0.4
321
0.4
355
3.7
797
2.1
319
1.0
000
20.0
764
0.2
230
0.4
779
1.1
225
1.2
951
2.6
659
0.6
798
1.3
254
Current Data ParametersNAME Sample-8866-5-DiMeOBn_2020-03-03_Acetone-d6EXPNO 2
PROCNO 1
F2 - Acquisition Parameters
Date_ 20200303Time 17.21INSTRUM spect
PROBHD 5 mm PABBO BB-PULPROG zgTD 131072
SOLVENT AcetoneNS 64DS 4
SWH 12626.263 HzFIDRES 0.096331 HzAQ 5.1904511 sec
RG 4DW 39.600 usecDE 6.50 usec
TE 298.2 KD1 20.00000000 secTD0 1
======== CHANNEL f1 ========SFO1 700.0842005 MHz
NUC1 1HP1 15.83 usecPLW1 26.00000000 W
F2 - Processing parametersSI 262144
SF 700.0800301 MHzWDW EMSSB 0
LB 0.10 HzGB 0PC 1.00
Sample:qNMR
8866-5 (0.1345 g) + 1,4-dimethoxybenzene (0.0725 g, internal standard, 99+% purity) in acetone-d6
1H
TM
S
Aceto
ne-d
5-
1,4
-dim
eth
oxybenzene
1,4
-dim
eth
oxybenzene
6.66.76.86.97.07.17.27.37.47.57.67.77.87.98.08.18.28.3 ppm
6.822
7.203
7.214
7.283
7.294
7.304
7.316
7.327
7.337
7.343
7.354
7.370
7.381
7.392
7.467
7.475
7.477
7.477
7.485
7.486
7.488
7.588
7.599
7.609
8.044
8.046
8.056
8.057
20.0
764
0.2
230
0.4
779
1.1
225
1.2
951
2.6
659
0.6
798
1.3
254
Sample:qNMR
8866-5 (0.1345 g) + 1,4-dimethoxybenzene (0.0725 g, internal standard, 99+% purity) in acetone-d6
1H
Expansion
Benzyl benzoate
Benzyl benzoate
Benzyl benzoate
Benzyl benzoate
Benzyl benzoate
12
6
3
54
O
O
1
6
2
5
3
4
Benzyl benzoate
1,4
-dim
eth
oxybenzene
1,4-Dimethoxybenzene
1
6
2
5
3
4
O
O
Benzyl alc
ohol
Benzyl alc
ohol
OH1
6
2
5
3
4
Benzyl alcohol
3.33.43.53.63.73.83.94.04.14.24.34.44.54.64.74.84.95.05.15.25.35.45.55.65.75.85.96.06.1 ppm
3.317
3.568
3.574
3.702
4.046
4.057
4.067
4.077
4.163
4.171
4.180
4.188
4.319
4.324
4.336
4.341
4.579
4.591
4.603
4.627
5.275
5.326
5.341
5.349
5.358
5.431
5.436
5.446
5.456
5.463
5.473
5.483
5.488
5.618
0.5
435
1.1
810
30.3
583
2.1
742
0.8
045
0.7
686
1.0
229
0.4
321
0.4
355
3.7
797
2.1
319
1.0
000
Sample:qNMR
8866-5 (0.1345 g) + 1,4-dimethoxybenzene (0.0725 g, internal standard, 99+% purity) in acetone-d6
1H
Expansion
Testo
ste
rone e
nanth
ate
C
H-4
Ric
inole
in -
CH
=C
H-
Benzyl benzoate
CH
2
Eth
yl ole
ate
C
H=
CH
Gly
cery
l C
H-O
Benzyl alc
ohol
CH
2
Testo
ste
rone e
nanth
ate
C
H-1
7
Eth
yl ole
ate
O
-CH
2
1,4
-dim
eth
oxybenzene
Gly
cery
l C
H2a-O
Gly
cery
l C
H2b-O
Ric
inole
in C
H-O
H
0.70.80.91.01.11.21.31.41.51.61.71.81.92.02.12.22.32.42.52.62.72.8 ppm
0.842
0.873
0.880
0.883
0.966
0.971
0.985
0.990
1.040
1.050
1.056
1.177
1.183
1.193
1.203
1.285
1.302
1.309
1.454
1.460
1.465
1.472
1.475
1.481
1.487
1.490
1.494
1.501
1.506
1.536
1.541
1.547
1.556
1.566
1.577
1.588
1.599
1.605
1.621
1.626
1.636
1.640
1.646
1.733
1.738
1.743
1.751
1.756
1.801
1.819
1.969
1.974
1.976
1.981
1.989
1.993
1.996
2.000
2.019
2.021
2.024
2.028
2.038
2.048
2.060
2.069
2.105
2.114
2.125
2.170
2.176
2.189
2.199
2.207
2.216
2.231
2.238
2.249
2.259
2.265
2.271
2.276
2.281
2.287
2.290
2.297
2.301
2.307
2.312
2.317
2.328
2.336
2.350
2.352
2.357
2.359
2.374
2.381
2.392
2.394
2.400
2.402
3.1
195
10.7
422
1.0
430
0.9
291
7.4
072
49.6
052
3.3
092
10.3
516
0.9
496
0.9
452
1.2
267
7.5
365
1.1
941
10.7
480
1.9
951
0.2
380
Sample:qNMR
8866-5 (0.1345 g) + 1,4-dimethoxybenzene (0.0725 g, internal standard, 99+% purity) in acetone-d6
Aceto
ne-d
5-
Testo
ste
rone e
nanth
ate
C
H2-7
a
Testo
ste
rone e
nanth
ate
C
H2-1
2a
Testo
ste
rone e
nanth
ate
C
H2-1
6b
Testo
ste
rone e
nanth
ate
C
H2-1
1b
Testo
ste
rone e
nanth
ate
C
H-1
4
Testo
ste
rone e
nanth
ate
C
H2-7
b
Testo
ste
rone e
nanth
ate
C
H-9
Testo
ste
rone e
nanth
ate
C
H2-1
2b
Testo
ste
rone e
nanth
ate
C
H3-1
8
Eth
yl ole
ate
C
H3
Ric
inole
in
Testo
ste
rone e
nanth
ate
C
H3-1
9
Eth
yl ole
ate
Eth
yl ole
ate
O
-CH
2-C
H3
Ric
inole
in
Eth
yl ole
ate
Ric
inole
in
Testo
ste
rone e
nanth
ate
C
H2-1
a
Testo
ste
rone e
nanth
ate
C
H2-2
a,
CH
2-6
a
Testo
ste
rone e
nanth
ate
C
H2-2
b
Testo
ste
rone e
nanth
ate
C
H2-1
6a
Testo
ste
rone e
nanth
ate
C
H2-6
b
Eth
yl ole
ate
O
-CH
2
Eth
yl ole
ateR
icin
ole
in
Ric
inole
in
1H
Expansion
210 200 190 180 170 160 150 140 130 120 110 100 90 80 70 60 50 40 30 20 10 0 ppm
14.368
14.522
17.504
21.151
23.093
23.246
23.932
25.488
25.519
25.563
25.683
26.409
27.688
27.715
27.944
27.954
28.111
32.131
32.213
32.539
32.603
33.051
34.290
34.388
34.510
34.722
35.960
36.294
36.409
37.380
37.732
39.131
43.117
50.832
54.506
55.687
60.253
62.621
64.551
66.984
69.760
71.486
82.553
115.202
124.250
127.149
127.165
127.189
127.396
128.639
128.668
128.764
128.794
129.216
129.242
130.137
130.374
130.453
130.517
130.551
131.012
131.751
131.769
133.782
137.242
143.235
154.587
166.391
170.464
172.860
173.134
173.333
173.384
197.942
205.832
Current Data ParametersNAME Sample-8866-5-DiMeOBn_2020-03-03_Acetone-d6EXPNO 4
PROCNO 1
F2 - Acquisition Parameters
Date_ 20200303Time 17.58INSTRUM spect
PROBHD 5 mm PABBO BB-PULPROG zgpg30TD 65536
SOLVENT AcetoneNS 256DS 4
SWH 41666.668 HzFIDRES 0.635783 HzAQ 0.7864320 sec
RG 2050DW 12.000 usecDE 7.71 usec
TE 298.1 KD1 2.00000000 secD11 0.03000000 sec
TD0 1
======== CHANNEL f1 ========
SFO1 176.0537397 MHzNUC1 13CP1 9.57 usec
PLW1 60.00000000 W
======== CHANNEL f2 ========
SFO2 700.0828003 MHzNUC2 1HCPDPRG[2 waltz16
PCPD2 65.00 usecPLW2 26.00000000 WPLW12 1.47850001 W
PLW13 0.62465000 W
F2 - Processing parameters
SI 262144SF 176.0351356 MHzWDW EM
SSB 0LB 1.00 HzGB 0
PC 1.40
210 200 190 180 170 160 150 140 130 120 110 100 90 80 70 60 50 40 30 20 10 0 ppm
Sample:qNMR sample
8866-5 (0.1345 g) + 1,4-dimethoxybenzene (0.0725 g, internal standard, 99+% purity) in acetone-d6
Aceto
ne-d
6
Aceto
ne-d
6
1,4
-dim
eth
oxybenzene
1,4
-dim
eth
oxybenzene
1,4
-dim
eth
oxybenzene
APT
13C{
1H}
C,CH2 ↑
↓ CH,CH3
165170175180185190195200205 ppm
166.391
170.464
172.860
173.134
173.333
173.384
197.942
205.832
165170175180185190195200205 ppm
Sample:qNMR sample
8866-5 (0.1345 g) + 1,4-dimethoxybenzene (0.0725 g, internal standard, 99+% purity) in acetone-d6
Aceto
ne-d
6
Testo
ste
rone e
nanth
ate
C
-3
13
149810
171211
15
16
756
1
4
2
3H
H
H
O
O
1
2 3
4 5
6 7
O
Testosterone enanthate
18
19
Testo
ste
rone e
nanth
ate
C
-5
Benzyl benzoate
CO
O
Testo
ste
rone e
nanth
ate
C
-1'
Eth
yl ole
ate
C
OO
Ric
inole
in C
OO
APT
13C{
1H}
C,CH2 ↑
↓ CH,CH3
115120125130135140145150155 ppm
115.202
124.250
127.149
127.165
127.189
127.396
128.639
128.668
128.764
128.794
129.216
129.242
130.137
130.374
130.453
130.517
130.551
131.012
131.751
131.769
133.782
137.242
143.235
154.587
115120125130135140145150155 ppm
Sample:qNMR sample
8866-5 (0.1345 g) + 1,4-dimethoxybenzene (0.0725 g, internal standard, 99+% purity) in acetone-d6
1,4
-dim
eth
oxybenzene 1,4
1,4
-dim
eth
oxybenzene 2,3
,5,6
Testo
ste
rone e
nanth
ate
C
H-4
Benzyl benzoate
1
4
Benzyl benzoate
Benzyl benzoate
Benzyl benzoate
Benzyl benzoate
1
Benzyl benzoate
Ric
inole
in C
=C
Eth
yl ole
ate
C
=C
Benzyl alc
ohol
1 6
2
Benzyl alc
ohol
4
Benzyl alc
ohol
APT
13C{
1H}
C,CH2 ↑
↓ CH,CH3
455055606570758085 ppm
43.117
50.832
54.506
55.687
60.253
62.621
64.551
66.984
69.760
71.486
82.553
455055606570758085 ppm
Sample:qNMR sample
8866-5 (0.1345 g) + 1,4-dimethoxybenzene (0.0725 g, internal standard, 99+% purity) in acetone-d6
Testo
ste
rone e
nanth
ate
C
H-1
7
Testo
ste
rone e
nanth
ate
C
H-9
Testo
ste
rone e
nanth
ate
C
H-1
4
Testo
ste
rone e
nanth
ate
C
-13
2×
OM
e
1,4
-dim
eth
oxybenzene
Benzyl benzoate
CH
2
Eth
yl ole
ate
O
-CH
2
Gly
ce
ryl C
H2-1
,3
Ric
inole
in C
H-O
H
Gly
cery
l C
H-2
Benzyl alc
ohol
CH
2
APT
13C{
1H}
C,CH2 ↑
↓ CH,CH3
15202530354045 ppm
12.327
14.277
14.345
14.368
14.522
17.504
21.151
23.093
23.246
23.932
25.488
25.519
25.563
25.683
26.409
27.688
27.715
27.944
27.954
28.111
32.131
32.213
32.539
32.603
33.051
34.290
34.388
34.510
34.722
35.960
36.294
36.409
37.380
37.732
39.131
43.117
15202530354045 ppm
Sample:qNMR sample
8866-5 (0.1345 g) + 1,4-dimethoxybenzene (0.0725 g, internal standard, 99+% purity) in acetone-d6
APT
13C{
1H}
C,CH2 ↑
↓ CH,CH3
Aceto
ne-d
6
10.0 9.5 9.0 8.5 8.0 7.5 7.0 6.5 6.0 5.5 5.0 4.5 4.0 3.5 3.0 2.5 2.0 1.5 1.0 0.5 0.0 ppm
0.792
0.841
0.846
0.851
0.856
0.861
0.866
1.145
1.159
1.169
1.179
1.232
1.246
1.280
1.291
1.301
1.310
1.319
1.328
1.336
1.341
1.345
1.354
1.360
1.498
1.509
1.519
1.528
1.568
1.580
1.585
1.594
1.607
1.956
1.963
1.971
1.973
1.981
1.990
2.058
2.068
2.077
2.235
2.246
2.249
2.254
2.257
2.259
2.265
2.269
2.275
2.370
2.384
2.386
2.391
2.503
2.505
2.508
2.511
2.513
3.326
4.022
4.032
4.042
4.052
4.350
4.357
4.498
4.506
4.524
4.536
4.537
4.548
5.308
5.315
5.322
5.362
5.630
7.315
7.321
7.357
7.367
7.399
7.408
7.410
7.420
7.471
7.472
7.482
7.484
7.524
7.535
7.536
7.546
7.657
7.667
8.001
8.003
8.006
8.011
8.013
8.015
3.3
156
7.7
752
1.1
041
1.1
140
1.1
725
4.0
832
2.5
628
38.6
058
1.2
913
6.2
573
3.1
611
1.0
805
1.0
279
5.4
886
2.8
311
1.1
897
6.2
667
2.0
639
1.3
435
0.1
248
0.7
353
0.8
575
1.3
126
0.6
032
0.5
966
0.8
380
0.6
114
1.0
110
0.2
990
0.3
066
4.9
207
1.0
000
0.2
997
1.1
595
0.8
485
1.6
875
1.6
778
1.6
882
0.8
379
1.6
603
Current Data ParametersNAME Sample-8866-5_2020-02-22_DMSO-d6EXPNO 2
PROCNO 1
F2 - Acquisition Parameters
Date_ 20200223Time 10.19INSTRUM spect
PROBHD 5 mm PABBO BB-PULPROG zg30TD 65536
SOLVENT DMSONS 64DS 2
SWH 12626.263 HzFIDRES 0.192661 HzAQ 2.5952256 sec
RG 25.4DW 39.600 usecDE 6.50 usec
TE 298.1 KD1 2.00000000 secTD0 1
======== CHANNEL f1 ========SFO1 700.0850406 MHz
NUC1 1HP1 15.50 usecPLW1 26.00000000 W
F2 - Processing parametersSI 262144
SF 700.0800000 MHzWDW EMSSB 0
LB 0.10 HzGB 0PC 1.00
1H
Qualitative analysisSample: 8866 5, in DMSO-d6+25 °C
DM
SO
-d5
-
TM
S
H O 2
7.107.157.207.257.307.357.407.457.507.557.607.657.707.757.807.857.907.958.008.058.108.158.208.258.308.35 ppm
7.216
7.222
7.228
7.315
7.321
7.344
7.346
7.348
7.354
7.357
7.359
7.365
7.367
7.369
7.399
7.401
7.408
7.410
7.417
7.420
7.471
7.472
7.482
7.484
7.524
7.527
7.535
7.536
7.544
7.546
7.655
7.657
7.658
7.666
7.667
7.669
7.676
7.678
7.680
8.001
8.003
8.006
8.011
8.013
8.015
8.017
0.2
997
1.1
595
0.8
485
1.6
875
1.6
778
1.6
882
0.8
379
1.6
603
Qualitative analysisSample: 8866 5, in DMSO-d6+25 °C
1H
Expansion
12
6
3
54
O
O
1
6
2
5
3
4
Benzyl benzoate
OH1
6
2
5
3
4
Benzyl alcohol
Benzyl benzoate
Benzyl benzoate
Benzyl benzoate
Benzyl benzoate
Benzyl benzoate
Benzyl benzoate
Benzyl alc
ohol
Benzyl alc
ohol
3.33.43.53.63.73.83.94.04.14.24.34.44.54.64.74.84.95.05.15.25.35.45.55.65.75.85.96.06.1 ppm
3.326
3.401
3.409
3.416
3.423
4.022
4.032
4.042
4.052
4.106
4.115
4.123
4.132
4.254
4.260
4.272
4.277
4.350
4.357
4.498
4.506
4.524
4.536
4.537
4.548
5.151
5.159
5.167
5.188
5.194
5.199
5.293
5.301
5.308
5.315
5.322
5.329
5.338
5.348
5.350
5.362
5.370
5.372
5.374
5.391
5.401
5.411
5.416
5.427
5.630
0.7
353
0.8
575
1.3
126
0.6
032
0.5
966
0.8
380
0.6
114
1.0
110
0.2
990
0.3
066
4.9
207
1.0
000
Qualitative analysisSample: 8866 5, in DMSO-d6+25 °C
1H
Expansion
H O 2
Testo
ste
rone e
nanth
ate
C
H-4
Testo
ste
rone e
nanth
ate
C
H-1
7
Benzyl alc
ohol
Benzyl benzoate
Benzyl alc
ohol
CH
2
OH
CH
2
OR
OR
OR
Glyceryl
Gly
cery
l C
H-2
Gly
cery
l C
H2-1
a, C
H2-3
a
Gly
cery
l C
H2-1
b, C
H2-3
b
1
2
3
Testo
ste
rone e
nanth
ate
C
H-1
7
12
6
3
54
O
O
1
6
2
5
3
4
Benzyl benzoate
OH1
6
2
5
3
4
Benzyl alcohol
Eth
yl ole
ate
O
-CH
2
Ric
inole
in -
OH
Ric
inole
in C
H-O
H
Eth
yl ole
ate
-
CH
=C
H-
Ric
inole
in -
CH
=C
H-
0.70.80.91.01.11.21.31.41.51.61.71.81.92.02.12.22.32.42.52.62.72.8 ppm
0.792
0.841
0.846
0.851
0.856
0.861
0.866
0.879
0.897
0.901
0.912
0.918
0.941
0.956
1.050
1.059
1.060
1.066
1.076
1.131
1.145
1.159
1.169
1.179
1.232
1.246
1.280
1.291
1.301
1.310
1.319
1.322
1.328
1.336
1.341
1.345
1.354
1.360
1.442
1.444
1.461
1.498
1.509
1.519
1.528
1.564
1.568
1.573
1.580
1.585
1.594
1.600
1.607
1.612
1.659
1.663
1.672
1.676
1.770
1.788
1.937
1.941
1.944
1.948
1.956
1.963
1.971
1.973
1.981
1.990
2.049
2.058
2.064
2.068
2.077
2.085
2.095
2.143
2.162
2.167
2.227
2.230
2.235
2.246
2.249
2.254
2.257
2.259
2.265
2.269
2.275
2.362
2.370
2.384
2.386
2.391
2.408
2.503
2.505
2.508
2.511
2.513
3.3
156
7.7
752
1.1
041
1.1
140
1.1
725
4.0
832
2.5
628
38.6
058
1.2
913
6.2
573
3.1
611
1.0
805
1.0
279
5.4
886
2.8
311
1.1
897
6.2
667
2.0
639
1.3
435
0.1
248
Qualitative analysisSample: 8866 5, in DMSO-d6+25 °C
1H
Expansion
DM
SO
-d5
-
Testo
ste
rone e
nanth
ate
C
H2-2
a, C
H2-6
a
Testo
ste
rone e
nanth
ate
C
H2-6
b
Testo
ste
rone e
nanth
ate
C
H2-2
b
Testo
ste
rone e
nanth
ate
C
H2-1
6a
Testo
ste
rone e
nanth
ate
C
H2-1
a
Testo
ste
rone e
nanth
ate
C
H2-7
a
Testo
ste
rone e
nanth
ate
C
H2-1
2a
Testo
ste
rone e
nanth
ate
C
H2-2
'
Testo
ste
rone e
nanth
ate
C
H2-1
b, C
H2-1
5a, C
H-8
Testo
ste
rone e
nanth
ate
C
H2-1
6b
Testo
ste
rone e
nanth
ate
C
H2-1
1b
Testo
ste
rone e
nanth
ate
C
H2-1
5b
Testo
ste
rone e
nanth
ate
C
H2-3
', C
H2-1
1a
Testo
ste
rone e
nanth
ate
C
H3-1
9
Testo
ste
rone e
nanth
ate
C
H2-4
', C
H2-5
', C
H2-6
'
Testo
ste
rone e
nanth
ate
C
H2-1
2b
Testo
ste
rone e
nanth
ate
C
H-1
4
Testo
ste
rone e
nanth
ate
C
H2-7
b
Testo
ste
rone e
nanth
ate
C
H-9
Testo
ste
rone e
nanth
ate
C
H3-1
8
Testo
ste
rone e
nanth
ate
C
H3-7
'
Eth
yl ole
ate
O
-CH
2-C
H3
210 200 190 180 170 160 150 140 130 120 110 100 90 80 70 60 50 40 30 20 10 0 ppm
24.433
24.558
25.208
26.559
26.574
26.606
26.832
27.108
28.096
28.422
28.447
28.464
28.547
28.571
28.629
28.722
28.874
28.933
29.058
29.084
29.125
30.893
31.137
31.306
31.394
31.874
33.310
33.487
33.557
33.727
34.690
35.133
35.156
36.183
36.504
38.128
42.054
49.505
53.078
59.539
61.755
62.884
66.131
68.732
69.762
81.483
123.205
126.363
126.540
126.616
126.629
127.912
127.966
128.064
128.478
128.753
129.183
129.515
129.560
129.585
130.210
130.259
133.379
136.104
142.525
165.519
170.496
171.976
172.300
172.617
172.686
197.764
Current Data ParametersNAME Sample-8866-5_2020-02-22_DMSO-d6EXPNO 4
PROCNO 1
F2 - Acquisition Parameters
Date_ 20200222Time 19.25INSTRUM spect
PROBHD 5 mm PABBO BB-PULPROG zgpg30TD 65536
SOLVENT DMSONS 2048DS 4
SWH 41666.668 HzFIDRES 0.635783 HzAQ 0.7864320 sec
RG 2050DW 12.000 usecDE 7.71 usec
TE 298.3 KD1 2.00000000 secD11 0.03000000 sec
TD0 1
======== CHANNEL f1 ========
SFO1 176.0537397 MHzNUC1 13CP1 9.57 usec
PLW1 60.00000000 W
======== CHANNEL f2 ========
SFO2 700.0828003 MHzNUC2 1HCPDPRG[2 waltz16
PCPD2 65.00 usecPLW2 26.00000000 WPLW12 1.47850001 W
PLW13 0.62465000 W
F2 - Processing parameters
SI 262144SF 176.0353415 MHzWDW EM
SSB 0LB 0.50 HzGB 0
PC 1.40
210 200 190 180 170 160 150 140 130 120 110 100 90 80 70 60 50 40 30 20 10 0 ppm
APT
Qualitative analysisSample: 8866 5, in DMSO-d6+25 °C
13C{
1H}
C,CH2 ↑
↓ CH,CH3
DM
SO
-d6
-
165170175180185190195200 ppm
165.519
170.496
171.976
172.300
172.617
172.686
197.764
165170175180185190195200 ppm
APT
Qualitative analysisSample: 8866 5, in DMSO-d6+25 °C
13C{
1H}
C,CH2 ↑
↓ CH,CH3
Expansion
Benzyl benzoate
CO
O
Testo
ste
rone e
nanth
ate
C
-3
Testo
ste
rone e
nanth
ate
C
-1'
Testo
ste
rone e
nanth
ate
C
-5
12
6
3
54
O
O
1
6
2
5
3
4
Benzyl benzoate
13
149810
171211
15
16
756
1
4
2
3H
H
H
O
O
1
2 3
4 5
6 7
O
Testosterone enanthate
18
19
Fatty a
cid
resid
ueF
att
y a
cid
resid
ue
Ric
inole
in C
OO
'
123124125126127128129130131132133134135136137138139140141142143144 ppm
123.205
126.363
126.540
126.616
126.629
127.912
127.966
128.064
128.478
128.753
129.183
129.515
129.560
129.585
130.210
130.259
133.379
136.104
142.525
123124125126127128129130131132133134135136137138139140141142143144 ppm
APT
Qualitative analysisSample: 8866 5, in DMSO-d6+25 °C
13C{
1H}
C,CH2 ↑
↓ CH,CH3
Expansion B
enzyl benzoate
1
4
Benzyl benzoate
Benzyl alc
ohol
1
12
6
3
54
O
O
1
6
2
5
3
4
Benzyl benzoate
OH1
6
2
5
3
4
Benzyl alcohol
Testo
ste
rone e
nanth
ate
C
H-4
Benzyl benzoate
62
Benzyl benzoate
53
Benzyl benzoate
4
1
Benzyl benzoate
2
6
Benzyl benzoate
Benzyl benzoate
3
5
62
Benzyl alc
ohol
4
Benzyl alc
ohol
Benzyl alc
ohol
5
3
Ric
inole
in C
=C
Eth
yl ole
ate
C
=C
455055606570758085 ppm
42.054
49.505
53.078
59.539
61.755
62.884
66.131
68.732
69.762
81.483
455055606570758085 ppm
APT
Qualitative analysisSample: 8866 5, in DMSO-d6+25 °C
13C{
1H}
C,CH2 ↑
↓ CH,CH3
Expansion
Testo
ste
rone e
nanth
ate
C
H-1
7
Testo
ste
rone e
nanth
ate
C
H-9
Testo
ste
rone e
nanth
ate
C
H-1
4
Testo
ste
rone e
nanth
ate
C
-13
Benzyl benzoate
Benzyl alc
ohol
CH
2
CH
2
Gly
cery
l C
H-2
Gly
cery
l C
H2-1
,3
OR
OR
OR
Glyceryl
OH1
6
2
5
3
4
Benzyl alcohol
13
149810
171211
15
16
756
1
4
2
3H
H
H
O
O
1
2 3
4 5
6 7
O
Testosterone enanthate
18
19
12
6
3
54
O
O
1
6
2
5
3
4
Benzyl benzoate
Eth
yl ole
ate
O
-CH
2
Ric
inole
in C
H-O
H
15202530354045 ppm
11.803
13.813
13.865
14.055
16.831
20.071
21.954
22.104
23.003
24.379
24.433
24.558
25.208
26.559
26.574
26.606
26.832
27.108
28.096
28.422
28.447
28.464
28.547
28.571
28.629
28.722
28.874
28.933
29.058
29.084
29.125
30.893
31.137
31.306
31.394
31.874
33.310
33.487
33.557
33.727
34.690
35.133
35.156
36.183
36.504
38.128
42.054
15202530354045 ppm
APT
Qualitative analysisSample: 8866 5, in DMSO-d6+25 °C
13C{
1H}
C,CH2 ↑
↓ CH,CH3
Expansion
DM
SO
-d6
-
Testo
ste
rone e
nanth
ate
C
-13
Testo
ste
rone e
nanth
ate
C
-10
Testo
ste
rone e
nanth
ate
C
H2-1
2
Testo
ste
rone e
nanth
ate
C
H2-1
Testo
ste
rone e
nanth
ate
C
H-8
Testo
ste
rone e
nanth
ate
C
H2-2
'T
esto
ste
rone e
nanth
ate
C
H2-2
Testo
ste
rone e
nanth
ate
C
H2-6
Testo
ste
rone e
nanth
ate
C
H2-7
Testo
ste
rone e
nanth
ate
C
H2-4
'
Testo
ste
rone e
nanth
ate
C
H2-1
6
Testo
ste
rone e
nanth
ate
C
H2-3
'
Testo
ste
rone e
nanth
ate
C
H2-5
'
Testo
ste
rone e
nanth
ate
C
H2-6
'
Testo
ste
rone e
nanth
ate
C
H2-1
5
Testo
ste
rone e
nanth
ate
C
H2-1
1
Testo
ste
rone e
nanth
ate
C
H3-1
9
Testo
ste
rone e
nanth
ate
C
H3-1
8
Testo
ste
rone e
nanth
ate
C
H3-7
'
15202530354045 ppm
11.803
13.813
13.865
14.055
16.831
20.071
21.954
22.104
23.003
24.379
24.433
24.558
25.208
26.559
26.574
26.606
26.832
27.108
28.096
28.422
28.447
28.464
28.547
28.571
28.629
28.722
28.874
28.933
29.058
29.084
29.125
30.893
31.137
31.306
31.394
31.874
33.310
33.487
33.557
33.727
34.690
35.133
35.156
36.183
36.504
38.128
42.054
15202530354045 ppm
ComparisonSample: 8866 5, in DMSO-d6+25 °C
Sample:
5134 1, in DMSO-d6