Post on 18-Aug-2020
transcript
MC1227
p-Acetamidophenol, [ring-14C(U)]-
Lot 198-185-079-A-20080611-DRE
A) All chromatograms were run using the HPLC method described on the Product Data Sheet.
Concentrations and volumes:
Standard solution concentration was 1.0 mg/mL.
p-Acetamidophenol, [ring-14C(U)]- concentration was 94.0 µCi/mL. Volume of standard alone injection was 1.0 µL.
Volume of p-Acetamidophenol, [ring-14C(U)]- alone injection was 1.0 µL.
Co-injection solution consisted of 1.0 µL p-Acetamidophenol, [ring-14C(U)]- + 1.0 µL standard.
Volume of co-injection was 2.0 µL.
Volume of blank injection was 1.0 µL.
B) Mass spectrometry- Positive Mode C) NMR
MC1227p-Acetamidophenol, [ring-14C(U)]-Lot 198-185-079-A-20080611-DRE
Chromatogram Info:
File Name : L:\int31241 File Created : 11/6/2013 9:29:18 AM
Origin : Acquired, Acquisition started 6/15/2012 3:21:15 PM Acquired Date : 6/15/2012 4:01:14 PM
Project : Test By : Administrator
Method : Unit3-40minrun By : Administrator
Description : Radiochemical trace of 14C material alone
Created : 6/12/2008 10:29 AM Modified : 11/6/2013 10:30 AM
Column : Detection : Radiochemical
Mobile Phase : Temperature :
Flow Rate : Pressure :
Note :
[min.]Time
10 20 30 40
[V]
Volta
ge
0.0
0.2
0.4
0.6
0.8
1.0
17.8
18
.5
18.9
21.6
22
.1
22.8
L:\ int 31241 - Unit 3 Radio
11/6/2013 10:31 AM Page 1 of 2Chromatogram L:\int31241.PRM
Result Table (Uncal - L:\int31241 - Unit 3 Radio)
CompoundName
Reten. Time[min]
Area[%]
Area[mV.s]
Height[mV]
Height[%]
Efficiency[th.pl]
1 17.813 0.06 12.019 0.954 0.104 34215.653
2 18.530 0.03 6.337 0.608 0.066 54591.755
3 18.870 99.55 20225.927 912.305 99.438 24004.860
4 21.583 0.06 11.612 0.415 0.045 526684.722
5 22.100 0.01 1.333 0.347 0.038 460342.582
6 22.800 0.30 60.809 2.833 0.309 44874.000
Total 100.00 20318.035 917.462 100.000
11/6/2013 10:31 AM Page 2 of 2Chromatogram L:\int31241.PRM
MC1227p-Acetamidophenol, [ring-14C(U)]-Lot 198-185-079-A-20080611-DRE
Chromatogram Info:
File Name : L:\int31241 File Created : 11/6/2013 9:29:18 AM
Origin : Acquired, Acquisition started 6/15/2012 3:21:15 PM Acquired Date : 6/15/2012 4:01:14 PM
Project : Test By : Administrator
Method : Unit3-40minrun By : Administrator
Description : UV trace of 14C material alone
Created : 6/12/2008 10:29 AM Modified : 11/6/2013 10:31 AM
Column : Detection : UV 255nm
Mobile Phase : Temperature :
Flow Rate : Pressure :
Note :
[min.]Time
10 20 30 40
[mV]
Volta
ge
0
50
100
150
18.5
22.4
L:\ int 31241 - Unit 3 UV
11/6/2013 10:31 AM Page 1 of 2Chromatogram L:\int31241.PRM
Result Table (Uncal - L:\int31241 - Unit 3 UV)
CompoundName
Reten. Time[min]
Area[%]
Area[mV.s]
Height[mV]
Height[%]
Efficiency[th.pl]
1 18.547 99.68 625.834 136.789 99.696 388906.694
2 22.437 0.32 2.013 0.418 0.304 474474.934
Total 100.00 627.847 137.207 100.000
11/6/2013 10:31 AM Page 2 of 2Chromatogram L:\int31241.PRM
MC1227p-Acetamidophenol, [ring-14C(U)]-Lot 198-185-079-A-20080611-DRE
Chromatogram Info:
File Name : L:\int31243 File Created : 11/6/2013 9:29:18 AM
Origin : Acquired, Acquisition started 6/15/2012 5:16:19 PM Acquired Date : 6/15/2012 5:56:18 PM
Project : Test By : Administrator
Method : Unit3-40minrun By : Administrator
Description : UV trace of standard alone
Created : 6/12/2008 10:29 AM Modified : 11/6/2013 9:33 AM
Column : Detection : UV 255nm
Mobile Phase : Temperature :
Flow Rate : Pressure :
Note :
[min.]Time
10 20 30 40
[mV]
Volta
ge
0
200
400
600
800
18.6
L:\ int 31243 - Unit 3 UV
11/6/2013 10:32 AM Page 1 of 2Chromatogram L:\int31243.PRM
Result Table (Uncal - L:\int31243 - Unit 3 UV)
CompoundName
Reten. Time[min]
Area[%]
Area[mV.s]
Height[mV]
Height[%]
Efficiency[th.pl]
1 18.627 100.00 3292.044 699.594 100.000 392268.984
Total 100.00 3292.044 699.594 100.000
11/6/2013 10:32 AM Page 2 of 2Chromatogram L:\int31243.PRM
MC1227p-Acetamidophenol, [ring-14C(U)]-Lot 198-185-079-A-20080611-DRE
Chromatogram Info:
File Name : L:\int31244 File Created : 11/6/2013 9:29:19 AM
Origin : Acquired, Acquisition started 6/18/2012 9:57:33 AM Acquired Date : 6/18/2012 10:37:32 AM
Project : Test By : Administrator
Method : Unit3-40minrun By : Administrator
Description : Radiochemical trace of 14C material co-injected with standard
Created : 6/12/2008 10:29 AM Modified : 11/6/2013 10:33 AM
Column : Detection : Radiochemical
Mobile Phase : Temperature :
Flow Rate : Pressure :
Note :
[min.]Time
10 20 30 40
[V]
Volta
ge
0.0
0.2
0.4
0.6
0.8
1.0
17.7
18.8
20.6
22.5
22
.8
27.4
L:\ int 31244 - Unit 3 Radio
11/6/2013 10:34 AM Page 1 of 2Chromatogram L:\int31244.PRM
Result Table (Uncal - L:\int31244 - Unit 3 Radio)
CompoundName
Reten. Time[min]
Area[%]
Area[mV.s]
Height[mV]
Height[%]
Efficiency[th.pl]
1 17.663 0.04 9.669 1.026 0.105 67517.310
2 18.783 99.46 23615.341 974.408 99.319 21717.638
3 20.650 0.08 19.864 0.527 0.054 291651.932
4 22.483 0.05 11.435 0.987 0.101 52938.970
5 22.817 0.24 57.222 3.020 0.308 37679.097
6 27.370 0.12 29.446 1.120 0.114 19900.351
Total 100.00 23742.978 981.088 100.000
11/6/2013 10:34 AM Page 2 of 2Chromatogram L:\int31244.PRM
MC1227p-Acetamidophenol, [ring-14C(U)]-Lot 198-185-079-A-20080611-DRE
Chromatogram Info:
File Name : L:\int31244 File Created : 11/6/2013 9:29:19 AM
Origin : Acquired, Acquisition started 6/18/2012 9:57:33 AM Acquired Date : 6/18/2012 10:37:32 AM
Project : Test By : Administrator
Method : Unit3-40minrun By : Administrator
Description : UV trace of 14C material co-injected with standard
Created : 6/12/2008 10:29 AM Modified : 11/6/2013 10:29 AM
Column : Detection : UV 255nm
Mobile Phase : Temperature :
Flow Rate : Pressure :
Note :
[min.]Time
10 20 30 40
[mV]
Volta
ge
0
200
400
600
800
18.4
19.5
19
.9
L:\ int 31244 - Unit 3 UV
11/6/2013 10:33 AM Page 1 of 2Chromatogram L:\int31244.PRM
Result Table (Uncal - L:\int31244 - Unit 3 UV)
CompoundName
Reten. Time[min]
Area[%]
Area[mV.s]
Height[mV]
Height[%]
Efficiency[th.pl]
1 18.427 99.56 4134.716 832.914 99.616 349784.428
2 19.520 0.21 8.731 1.901 0.227 474954.394
3 19.893 0.23 9.452 1.312 0.157 205326.028
Total 100.00 4152.898 836.126 100.000
11/6/2013 10:33 AM Page 2 of 2Chromatogram L:\int31244.PRM
MC1227p-Acetamidophenol, [ring-14C(U)]-Lot 198-185-079-A-20080611-DRE
Chromatogram Info:
File Name : L:\int31240 File Created : 11/6/2013 9:29:18 AM
Origin : Acquired, Acquisition started 6/15/2012 2:29:57 PM Acquired Date : 6/15/2012 3:09:56 PM
Project : Test By : Administrator
Method : Unit3-40minrun By : Administrator
Description : UV trace of blank injection
Created : 6/12/2008 10:29 AM Modified : 11/6/2013 9:30 AM
Column : Detection : UV 255nm
Mobile Phase : Temperature :
Flow Rate : Pressure :
Note :
[min.]Time
10 20 30 40
[mV]
Volta
ge
-10
0
10
20
30
L:\ int 31240 - Unit 3 UV
11/6/2013 10:34 AM Page 1 of 2Chromatogram L:\int31240.PRM
Result Table (Uncal - L:\int31240 - Unit 3 UV)
CompoundName
Reten. Time[min]
Area[%]
Area[mV.s]
Height[mV]
Height[%]
Efficiency[th.pl]
No peak to report
11/6/2013 10:34 AM Page 2 of 2Chromatogram L:\int31240.PRM
C:\Xcalibur\data\MC1227-20080611-DRE 6/15/2012 4:05:41 PM MC1227-20080611-DRE
RT: 0.00 - 9.00
0 1 2 3 4 5 6 7 8 9
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
4.77
0.484.59
4.183.860.76
3.53
3.30
2.62
2.32
2.16
NL:8.25E8
TIC F: MS MC1227-20080611-DRE
MC1227-20080611-DRE#31-70 RT: 0.39-0.89T: + c sid=-10.00 Q3MS [ 50.00-400.00]m/z= 189.60-214.65
m/z Intensity Relativem/z Intensity Relative
190.03 132798.1 0.25 192.27 132310.2 0.25 193.04 33481495.5 62.45 194.04 3831888.4 7.15 195.04 53609525.1 100.00 196.04 5721353.2 10.67 197.04 37235822.3 69.46 198.04 4621125.3 8.62 199.05 14375981.9 26.82 200.05 2248234.8 4.19 201.05 3236584.1 6.04 202.05 920277.7 1.72 203.05 509338.1 0.95 204.07 294611.2 0.55 208.00 126732.5 0.24 210.06 241195.5 0.45 211.03 134090.8 0.25 212.04 804222.2 1.50 213.06 257792.4 0.48 214.04 477326.6 0.89
MC1227-20080611-DRE #31-72 RT: 0.39-0.91 AV: 42 NL: 7.79E7T: + c sid=-10.00 Q3MS [ 50.00-400.00]
50 100 150 200 250 300 350 400
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
129.07
195.04
154.0588.11
83.08
307.00
321.96217.01 261.69396.97
MC1227-20080611-DRE #31-68 RT: 0.39-0.86 AV: 38 NL: 5.40E7T: + c sid=-10.00 Q3MS [ 50.00-400.00]
190 200 210 220 230 240 250
m/z
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
Relative Abundance
195.04
197.04
193.04
199.05
201.05217.01 242.18
235.97202.05 227.09186.15 251.05
98
76
54
32
1pp
m
2.094
6.7226.7456.751
7.2997.329
2.98
2.09
2.00
PC 1.00
GB 0
LB 0.00 Hz
SSB 0
WDW no
SF 300.1300000 MHz
SI 32768
SFO1 300.1318534 MHz
PL1 0.00 dB
P1 7.25 usec
NUC1 1H
======== CHANNEL f1 ========
TD0 1
D1 1.00000000 sec
TE 300.0 K
DE 6.50 usec
DW 92.400 usec
RG 645.1
AQ 6.0555763 sec
FIDRES 0.082569 Hz
SWH 5411.255 Hz
DS 2
NS 512
SOLVENT MeOD
TD 65536
PULPROG zg30
PROBHD 5 mm DUX 3H−1H
INSTRUM spect
Time 10.25
Date_ 20120712
PROCNO 1
EXPNO 1
NAME MC1227−20080611−DRE
Batch 20080611−DRE
MC1227 1H NMR in MeOD