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MT-1620
(R,S)-Warfarin, [phenyl-4-3H]-
Lot 194-090-0171-A-20090715-JG
A) All chromatograms were run using the HPLC method described on the Product Data Sheet.
Concentrations and volumes:
Standard solution concentration was 0.5 mg/ml.
(R,S)-Warfarin, [phenyl-4-3H]- concentration was 0.1 mCi/ml. Volume of standard alone injection was 2.0 µl.
Volume of (R,S)-Warfarin, [phenyl-4-3H]- alone injection was 2.0 µl.
Co-injection solution consisted of 2.0 µl (R,S)-Warfarin, [phenyl-4-3H]- + 2.0 µl standard.
Volume of co-injection was 4.0 µl.
Volume of blank injection was 2.0 µl.
B) Mass spectrometry – Negative mode
C) NMR
MT-1620(R,S)-Warfarin, [phenyl-4-3H]-
Lot 194-090-0171-A-20090715-JG
Chromatogram Info:
File Name : L:\int20532 File Created : 3/26/2014 4:26:33 PM
Origin : Acquired, Acquisition started 6/2/2010 11:02:04 AM Acquired Date : 6/2/2010 11:22:02 AM
Project : Test By : Administrator
Method : unit2-20minrun By : Administrator
Description : Radiochemical trace of 3H material alone
Created : 8/8/2007 9:12 AM Modified : 3/26/2014 4:35 PM
Column : Detection : Radiochemical
Mobile Phase : Temperature :
Flow Rate : Pressure :
Note :
[min.]Time
5 10 15 20
[mV]
Volta
ge
0
100
200
300
400
6.54
1
9.43
2
L:\ int 20532 - Unit 2 Radio
3/26/2014 4:35 PM Page 1 of 2Chromatogram L:\int20532.PRM
Result Table (Uncal - L:\int20532 - Unit 2 Radio)
CompoundName
Reten. Time[min]
Area[mV.s]
Height[mV]
Area[%]
Height[%]
Efficiency[th.pl]
Eff/l[t.p./m]
Symmetry/Tailing[-]
Response Factor
Resolution[-]
1 6.54 24.047 2.32 0.31 0.64 8199.12 163982.47 1.44
2 9.43 7739.467 359.96 99.69 99.36 4619.88 92397.56 1.18 6.9
Total 7763.515 362.28 100.00 100.00
3/26/2014 4:35 PM Page 2 of 2Chromatogram L:\int20532.PRM
MT-1620(R,S)-Warfarin, [phenyl-4-3H]-
Lot 194-090-0171-A-20090715-JG
Chromatogram Info:
File Name : L:\int20532 File Created : 3/26/2014 4:26:33 PM
Origin : Acquired, Acquisition started 6/2/2010 11:02:04 AM Acquired Date : 6/2/2010 11:22:02 AM
Project : Test By : Administrator
Method : unit2-20minrun By : Administrator
Description : UV trace of 3H material alone
Created : 8/8/2007 9:12 AM Modified : 3/26/2014 4:34 PM
Column : Detection : 308nm
Mobile Phase : Temperature :
Flow Rate : Pressure :
Note :
[min.]Time
5 10 15 20
[mV]
Volta
ge
-0.2
0.0
0.2
0.4
0.6
0.8
1.0
9.15
1
L:\ int 20532 - Unit 2 UV
3/26/2014 4:34 PM Page 1 of 2Chromatogram L:\int20532.PRM
Result Table (Uncal - L:\int20532 - Unit 2 UV)
CompoundName
Reten. Time[min]
Area[mV.s]
Height[mV]
Area[%]
Height[%]
Efficiency[th.pl]
Eff/l[t.p./m]
Symmetry/Tailing[-]
Response Factor
Resolution[-]
1 9.15 7.540 0.53 100.00 100.00 9021.11 180422.27 0.95
Total 7.540 0.53 100.00 100.00
3/26/2014 4:34 PM Page 2 of 2Chromatogram L:\int20532.PRM
MT-1620(R,S)-Warfarin, [phenyl-4-3H]-
Lot 194-090-0171-A-20090715-JG
Chromatogram Info:
File Name : L:\int20533 File Created : 3/26/2014 4:26:33 PM
Origin : Acquired, Acquisition started 6/2/2010 11:36:33 AM Acquired Date : 6/2/2010 11:56:32 AM
Project : Test By : Administrator
Method : unit2-20minrun By : Administrator
Description : UV trace of standard material alone
Created : 8/8/2007 9:12 AM Modified : 3/26/2014 4:35 PM
Column : Detection : UV 308nm
Mobile Phase : Temperature :
Flow Rate : Pressure :
Note :
[min.]Time
5 10 15 20
[mV]
Volta
ge
0
50
100
150
9.10
1
L:\ int 20533 - Unit 2 UV
3/26/2014 4:36 PM Page 1 of 2Chromatogram L:\int20533.PRM
Result Table (Uncal - L:\int20533 - Unit 2 UV)
CompoundName
Reten. Time[min]
Area[mV.s]
Height[mV]
Area[%]
Height[%]
Efficiency[th.pl]
Eff/l[t.p./m]
Symmetry/Tailing[-]
Response Factor
Resolution[-]
1 9.10 2035.613 143.59 100.00 100.00 9485.61 189712.21 0.94
Total 2035.613 143.59 100.00 100.00
3/26/2014 4:36 PM Page 2 of 2Chromatogram L:\int20533.PRM
MT-1620(R,S)-Warfarin, [phenyl-4-3H]-
Lot 194-090-0171-A-20090715-JG
Chromatogram Info:
File Name : L:\int20534 File Created : 3/26/2014 4:26:33 PM
Origin : Acquired, Acquisition started 6/2/2010 12:00:09 PM Acquired Date : 6/2/2010 12:20:07 PM
Project : Test By : Administrator
Method : unit2-20minrun By : Administrator
Description : Radiochemical trace of 3H material co-injected with standard
Created : 8/8/2007 9:12 AM Modified : 3/26/2014 4:37 PM
Column : Detection : Radiochemical
Mobile Phase : Temperature :
Flow Rate : Pressure :
Note :
[min.]Time
5 10 15 20
[mV]
Volta
ge
0
100
200
300
4009.
42
1 L:\ int 20534 - Unit 2 Radio
3/26/2014 4:37 PM Page 1 of 2Chromatogram L:\int20534.PRM
Result Table (Uncal - L:\int20534 - Unit 2 Radio)
CompoundName
Reten. Time[min]
Area[mV.s]
Height[mV]
Area[%]
Height[%]
Efficiency[th.pl]
Eff/l[t.p./m]
Symmetry/Tailing[-]
Response Factor
Resolution[-]
1 9.42 7863.387 368.90 100.00 100.00 4424.40 88487.94 1.10
Total 7863.387 368.90 100.00 100.00
3/26/2014 4:37 PM Page 2 of 2Chromatogram L:\int20534.PRM
MT-1620(R,S)-Warfarin, [phenyl-4-3H]-
Lot 194-090-0171-A-20090715-JG
Chromatogram Info:
File Name : L:\int20534 File Created : 3/26/2014 4:26:33 PM
Origin : Acquired, Acquisition started 6/2/2010 12:00:09 PM Acquired Date : 6/2/2010 12:20:07 PM
Project : Test By : Administrator
Method : unit2-20minrun By : Administrator
Description : UV trace of 3H material co-injected with standard
Created : 8/8/2007 9:12 AM Modified : 3/26/2014 4:38 PM
Column : Detection : UV 308nm
Mobile Phase : Temperature :
Flow Rate : Pressure :
Note :
[min.]Time
5 10 15 20
[mV]
Volta
ge
0
50
100
1509.
15
1L:\ int 20534 - Unit 2 UV
3/26/2014 4:38 PM Page 1 of 2Chromatogram L:\int20534.PRM
Result Table (Uncal - L:\int20534 - Unit 2 UV)
CompoundName
Reten. Time[min]
Area[mV.s]
Height[mV]
Area[%]
Height[%]
Efficiency[th.pl]
Eff/l[t.p./m]
Symmetry/Tailing[-]
Response Factor
Resolution[-]
1 9.15 1971.051 135.68 100.00 100.00 9021.11 180422.27 0.94
Total 1971.051 135.68 100.00 100.00
3/26/2014 4:38 PM Page 2 of 2Chromatogram L:\int20534.PRM
MT-1620(R,S)-Warfarin, [phenyl-4-3H]-
Lot 194-090-0171-A-20090715-JG
Chromatogram Info:
File Name : L:\int20530 File Created : 3/26/2014 4:26:33 PM
Origin : Acquired, Acquisition started 6/2/2010 9:46:26 AM Acquired Date : 6/2/2010 10:06:25 AM
Project : Test By : Administrator
Method : unit2-20minrun By : Administrator
Description : UV trace of blank injection
Created : 8/8/2007 9:12 AM Modified : 3/26/2014 4:38 PM
Column : Detection : UV 308nm
Mobile Phase : Temperature :
Flow Rate : Pressure :
Note :
[min.]Time
5 10 15 20
[mV]
Volta
ge
-2
0
2
4
L:\ int 20530 - Unit 2 UV
3/26/2014 4:38 PM Page 1 of 2Chromatogram L:\int20530.PRM
Result Table (Uncal - L:\int20530 - Unit 2 UV)
CompoundName
Reten. Time[min]
Area[mV.s]
Height[mV]
Area[%]
Height[%]
Efficiency[th.pl]
Eff/l[t.p./m]
Symmetry/Tailing[-]
Response Factor
Resolution[-]
No peak to report
3/26/2014 4:38 PM Page 2 of 2Chromatogram L:\int20530.PRM
C:\Xcalibur\data\MT1620-20090715-JG-MS 4/28/2010 9:34:51 AM MT1620-20090715-JG
RT: 0.00 - 2.00
0.0 0.5 1.0 1.5 2.0
Time (min)
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100
Relative Abundance
0.350.38
0.29
0.46
0.520.68
0.72 0.79
0.94 1.350.261.72
1.15 1.37
1.55 1.74
0.23
NL:7.67E7
TIC MS MT1620-20090715-JG-MS
MT1620-20090715-JG-MS#1-168 RT: 0.01-2.00T: - c NSI Full ms [50.00-700.00]m/z= 299.01-324.05
m/z Intensity Relativem/z Intensity Relative
306.85 67381.4 1.19 307.50 3859424.0 68.19 308.49 812116.9 14.35 309.45 5660192.4 100.00 310.48 1093874.5 19.33 311.51 430810.6 7.61 312.56 72463.1 1.28 313.59 14640.9 0.26 314.44 1961.1 0.03 315.12 5551.7 0.10 316.40 8922.3 0.16 317.02 161202.1 2.85 317.63 18955.6 0.33 318.49 6293.0 0.11 319.22 4349.9 0.08 321.28 5031.4 0.09 322.69 13896.8 0.25 323.20 18746.8 0.33
MT1620-20090715-JG-MS #1-168 RT: 0.01-2.00 AV: 168 NL: 5.66E6T: - c NSI Full ms [50.00-700.00]
100 200 300 400 500 600 700
m/z
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100
Relative Abundance
309.45
370.31
639.09384.87161.37 520.79252.50 656.61
MT1620-20090715-JG-MS #1-168 RT: 0.01-2.00 AV: 168 NL: 5.66E6T: - c NSI Full ms [50.00-700.00]
280 300 320 340
m/z
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100
Relative Abundance
309.45
307.50
310.48
311.51
317.02325.52 339.34 353.18305.61295.18281.38
98
76
54
32
1pp
m
7.2157.2397.263
1.00
PC 1.00
GB 0
LB 0.00 Hz
SSB 0
WDW no
SF 320.1305850 MHz
SI 32768
SFO1 320.1321857 MHz
PL1 2.00 dB
P1 10.00 usec
NUC1 3H
======== CHANNEL f1 ========
TD0 1
D1 2.00000000 sec
TE 300.0 K
DE 6.00 usec
DW 81.000 usec
RG 46341
AQ 1.3271540 sec
FIDRES 0.376760 Hz
SWH 6172.839 Hz
DS 2
NS 2549
SOLVENT MeOD
TD 16384
PULPROG zg
PROBHD 5 mm DUX 3H−1H
INSTRUM spect
Time 10.35
Date_ 20090717
PROCNO 1
EXPNO 1
NAME MT1620−20090715−JG
Batch 20090715−JG
MT1620 3H NMR in MeOD
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