figure 1. ft-ir spectra of reference standard...
TRANSCRIPT
Figures
82
Figure 1. FT-IR Spectra of reference standard Phenytoin
Figures
83
Figure 2. FT-IR spectra of working standard Phenytoin
Figures
84
Figure 3. FT-IR spectra of Benzil
Figures
85
Figure 4. FT-IR Spectra of reference standard Warfarin
Figures
86
Figure 5. FT-IR Spectra of working standard Warfarin
Figures
87
Figure 6. FT-IR Spectra of Benzalacetone
Figures
88
Figure 7. FT-IR spectra of reference standard d Nicergoline
Figures
89
Figure 8. FT-IR spectra of working standard Nicergoline
Figures
90
Figure 9. FT-IR spectra of 5-Bromo Nicotinic Acid
Figures
91
Figure 10. Typical chromatogram of standard Phenytoin and Benzil (10µg/ml)
Figures
92
Figure 11. Typical mass spectra of standard Phenytoin and Benzil (10µg/ml)
210.0 215.0 220.0 225.0 230.0 235.0 240.0 245.0 250.0 m/z0.0
2.5
5.0Inten. (x1,000)
25
120
9
Figures
93
Figure 12. Typical mass spectra of Phenytoin in scan negative mode.
200 210 220 230 240 250 260 270 m/z0.0
0.5
1.0
1.5
2.0
2.5
3.0Inten. (x100,000)
25
1
25
5
20
3
21
7
26
2
27
9
22
7
22
3
24
7
23
9
26
5
24
1
20
5
23
3
27
1
21
1
Figures
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Figure 13. Typical mass spectra of Phenytoin in SIM mode.
250.000 250.250 250.500 250.750 251.000 251.250 251.500 251.750 m/z0.00
0.25
0.50
0.75
1.00Inten. (x10,000)
25
1
Figures
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Figure 14. Typical mass spectra of Benzil in scan negative mode.
200 210 220 230 240 250 260 270 m/z0.0
1.0
2.0
3.0
4.0
5.0
6.0
Inten. (x1,000)
22
8
26
9
25
6
25
224
4
27
9
21
1
20
9
26
0
24
5
23
0
21
8
23
7
20
1
22
1
Figures
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Figure 15. Typical mass spectra of Benzil in SIM mode.
208.000 208.250 208.500 208.750 209.000 209.250 209.500 209.750 m/z0.00
0.25
0.50
0.75
1.00
1.25
1.50
Inten. (x10,000)
20
9
Figures
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Figure 16. Typical chromatogram of standard Warfarin and Benzalacetone.
Figures
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Figure 17. Typical chromatogram of Benzalacetone in formulation
Figures
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Figure 18. Typical chromatogram of Benzalacetone in bulk drug
Figures
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Figure 19. Typical mass spectra of Warfarin in scan mode.
285.0 290.0 295.0 300.0 305.0 310.0 315.0 320.0 325.0 330.0 335.0 340.0 345.0 m/z0.0
1.0
2.0
Inten. (x1,000,000)
30
9
31
1
34
7
33
1
34
3
32
5
34
1
29
1
31
5
28
9
33
7
29
9
29
7
28
4
32
0
30
4
Figures
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Figure 20. Typical mass spectra of Warfarin and Benzalacetone in SIM mode.
150.0 175.0 200.0 225.0 250.0 275.0 300.0 m/z0.00
0.25
0.50
0.75
1.00
Inten. (x10,000)
30
9
14
7
Figures
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Figure 21. Typical mass spectra of Benzalacetone in scan positive mode.
130 140 150 160 170 180 190 m/z0.0
2.5
5.0
Inten. (x10,000)
14
7
13
0
14
8
18
8
17
9
13
9
17
3
13
2
18
1
14
3
19
5
16
3
16
5
12
2
15
6
12
7
16
9
Figures
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Figure 22. Typical chromatogram of Standard Nicergoline and 5-Bromo Nicotinic Acid (10µg/ml)
Minutes
0 1 2 3 4 5 6 7 8 9 10
Volts
0.00
0.02
0.04
0.06
Volts
0.00
0.02
0.04
0.06
2.9
58
4.6
33
Detector A (277nm)validationassay001
Retention Time
Figures
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Figure 23. Typical chromatogram of Sample Nicergoline and 5-Bromo Nicotinic Acid
Minutes
0 1 2 3 4 5 6 7 8 9 10
Volts
0.00
0.02
0.04
0.06
Volts
0.00
0.02
0.04
0.06
2.317
2.600
2.800
4.650
Detector A (277nm)AlkaliI 24HrAlkali 24 Hr 001
Retention Time
Figures
105
Figure 24. Typical mass spectra of Nicergoline scan positive mode.
450 460 470 480 490 500 510 520 530 540 m/z0.0
2.5
5.0
7.5
Inten. (x100,000)
48
4
48
6
45
2
52
5
50
0
45
6
52
8
47
5
50
5
54
9
52
0
49
5
53
5
54
1
46
8
51
3
46
3
Figures
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Figure 25. Typical mass spectra of 5-Bromo Nicotinic Acid scan positive mode
175.0 200.0 225.0 250.0 275.0 300.0 325.0 m/z0.00
0.25
0.50
0.75
1.00
Inten. (x10,000)
27
2
31
3
24
3
20
2
28
4
29
9
25
6
21
3
33
2
26
3
32
2
34
5
30
3
23
3
19
1
18
3
15
8
16
2
22
9
17
8
.
Figures
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Figure 26. Calibration curve of Benzil
Figures
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Figure 27. Calibration curve of Benzalacetone
Figures
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Figure 28. Calibration curve of 5-Bromo Nicotinic Acid
Figures
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Figure 29. Genotoxicity study control (Hydroxylamine 8% v/v)
Figures
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Figure 30. Genotoxicity study for Benzil
Figures
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Figure 31. Genotoxicity study for Benzalacetone
Figures
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Figure 32. Genotoxicity Report For5-Bromo Nicotinic Acidin terms of concentration
Well - 1: Plasmid alone, Well - 2: Quercetin (Positive control), Well- 3 : Fenton’s reagent (-ve control), Well - 4 : 6.5 µg/ ml
sample solution, Well - 5 : 100 µg/ml sample solution, Well - 6: 200 µg/ml sample solution, Well- 7 : 300µg/ml sample
solution
6 7 2 1 3 4 5
Figures
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Figure 33. genotoxicity report for 5-Bromo Nicotinic Acidin terms of time
Well-1: Plasmid alone, Well-2: 2 hrs incubation , Well-3: 4 hrs incubation , Well-4: 6 hrs incubation , Well-5:124 hrs
incubation and Well-6: 24 hrs incubation ,
6 5 4 3 2 1