Ultisil PAH-Dextromethorphan HBr Analytical Method Development Report
Test Report
Chromatography conditions:
Column |
Welch Utisil PAH（4.6×250mm,5μm） |
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Mobile Phase |
Sodium sulfosuccinate dioctyl ester ammonium nitrate aqueous solution-acetonitrile (4:5) (glacial acetic acid to adjust pH = 2.0) |
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Column Temperature |
25℃ |
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Detector |
UV |
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Injection Volume |
20μL |
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Flow Rate |
1.0 ml/min |
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Detect wavelength |
280 nm |
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Elution procedure |
|
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Note |
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Chromatogram and Data:
- 1) Blank solvent analysis spectrum:
- 2) Analysis spectrum of main substance YMSF-7# control solution
Serial number |
Peak name |
Retention time (min) |
Peak Area(mAU*min) |
Relative peak area(%) |
S/N |
Resolution |
Number of plates(EP) |
Asymmetry |
1 |
YMSF-7# |
34.181 |
9.781 |
100.00 |
826.4 |
N.a. |
21154 |
1.02 |
Sum |
9.781 |
|
826.42 |
0.00 |
|
|
- 3) Impurity YMSF-7#-2 reference solution analysis spectrum:
Serial number |
Peak name |
Retention time (min) |
Peak Area |
Relative peak area(%) |
S/N |
Resolution |
Number of plates(EP) |
Asymmetry |
1 |
YMSF-7#-2 |
11.608 |
70.142 |
100.00 |
11850.8 |
N.a. |
11623 |
0.66 |
Sum |
70.142 |
|
11850.75 |
0.00 |
|
|
- 4) Impurity YMSF-6# control solution analysis spectrum:
Serial number |
Peak name |
Retention time (min) |
Peak Area |
Relative peak area(%) |
S/N |
Resolution |
Number of plates(EP) |
Asymmetry |
1 |
YMSF-6# |
14.966 |
58.293 |
100.00 |
7771.2 |
N.a. |
16438 |
1.31 |
Sum |
58.293 |
|
7771.19 |
0.00 |
|
|
- 5) Mixed control solution analysis spectrum:
Serial number |
Peak name |
Retention time (min) |
Peak Area |
Relative peak area(%) |
S/N |
Resolution |
Number of plates(EP) |
Asymmetry |
1 |
YMSF-7# -2 |
11.497 |
12.084 |
12.38 |
2046.0 |
8.72 |
17214 |
0.85 |
2 |
YMSF-6# |
15.052 |
9.595 |
9.83 |
1239.7 |
12.34 |
16634 |
1.03 |
3 |
YMSF-7#-3 |
21.862 |
48.258 |
49.45 |
4523.3 |
10.06 |
18652 |
0.98 |
4 |
YMSF-7#-4 |
29.215 |
9.429 |
9.66 |
696.0 |
3.33 |
20014 |
0.97 |
5 |
YMSF-7#-7 |
32.057 |
9.435 |
9.67 |
649.4 |
1.51 |
20882 |
1.01 |
6 |
YMSF-7# |
33.432 |
8.780 |
9.00 |
53.1 |
N.a. |
20420 |
0.98 |
Sum |
97.581 |
|
9727.43 |
35.95 |
|
|
3. Conclusion
Using Welch Ultisil PAH (4.6×250mm, 5μm) column to analyze the mixed control solution under this chromatographic condition, the separation degree between the main substance and the five impurities was not less than 1.5, which met the analysis requirements.