Ultisil XB-C8-Eribulin Mesylate Injection Analytical Method Development Report
Test Report
Chromatography conditions:
Column |
Welch Utisil XB-C8（4.6×150mm,3μm，300A） |
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Mobile Phase |
Phosphate buffer (pH=7.0)-acetonitrile (73:27) |
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Column Temperature |
30℃ |
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Detector |
UV |
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Injection Volume |
50μL |
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Flow Rate |
1 ml/min |
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Detect wavelength |
200 nm |
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Elution procedure |
|
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Note |
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Chromatogram and Data:
- 1) Blank solvent analysis spectrum:
Serial number |
Peak name |
Retention time (min) |
Peak Area(mAU*min) |
S/N |
Relative peak area(%) |
Resolution(EP) |
Number of plates(EP) |
Asymmetry(EP) |
Sum |
|
0.000 |
|
0.00 |
0.00 |
|
|
- 2) System suitability solution analysis spectrum full range
Serial number |
Peak name |
Retention time (min) |
Peak Area(mAU*min) |
S/N |
Relative peak area(%) |
Resolution(EP) |
Number of plates(EP) |
Asymmetry(EP) |
1 |
impA |
4.668 |
6.452 |
42.1 |
1.49 |
12.54 |
14973 |
1.24 |
2 |
ER |
10.557 |
404.741 |
496.4 |
93.77 |
10.16 |
2864 |
4.91 |
3 |
impD |
17.203 |
12.065 |
47.6 |
2.80 |
2.77 |
17320 |
1.25 |
4 |
impE |
18.682 |
6.963 |
18.4 |
1.61 |
12.84 |
18749 |
1.14 |
5 |
ImpG |
27.308 |
1.408 |
2.5 |
0.33 |
N.a. |
18576 |
1.08 |
Sum |
431.628 |
|
100.00 |
38.31 |
|
|
- 3) System suitability solution analysis spectrum magnification range:
Serial number |
Peak name |
Retention time (min) |
Peak Area(mAU*min) |
S/N |
Relative peak area(%) |
Resolution(EP) |
Number of plates(EP) |
Asymmetry(EP) |
1 |
impA |
4.668 |
6.452 |
42.1 |
1.49 |
12.54 |
14973 |
1.24 |
2 |
ER |
10.557 |
404.741 |
496.4 |
93.77 |
10.16 |
2864 |
4.91 |
3 |
impD |
17.203 |
12.065 |
47.6 |
2.80 |
2.77 |
17320 |
1.25 |
4 |
impE |
18.682 |
6.963 |
18.4 |
1.61 |
12.84 |
18749 |
1.14 |
5 |
ImpG |
27.308 |
1.408 |
2.5 |
0.33 |
N.a. |
18576 |
1.08 |
Sum |
431.628 |
|
100.00 |
38.31 |
|
|
- 4) Batch Verification 1303.02 Batch System Suitability Solution Analysis Spectrum:
Serial number |
Peak name |
Retention time (min) |
Peak Area(mAU*min) |
S/N |
Relative peak area(%) |
Resolution(EP) |
Number of plates(EP) |
Asymmetry(EP) |
1 |
impA |
4.665 |
6.460 |
40 .9 |
1.49 |
12.52 |
14968 |
1.22 |
2 |
ER |
10.543 |
405.781 |
482.4 |
93.75 |
10.14 |
2859 |
4.83 |
3 |
impD |
17.187 |
12.243 |
48.8 |
2.83 |
2.77 |
171780 |
1.26 |
4 |
impE |
18.663 |
7.041 |
19.3 |
1.63 |
13.00 |
18737 |
1.12 |
5 |
ImpG |
27.292 |
1.324 |
2.5 |
0.31 |
N.a. |
19311 |
1.07 |
Sum |
432.849 |
|
100.00 |
38.44 |
|
|
- 5) Batch Validation 1303.03 Batch System Suitability Solution Analysis Spectrum
Serial number |
Peak name |
Retention time (min) |
Peak Area(mAU*min) |
S/N |
Relative peak area(%) |
Resolution(EP) |
Number of plates(EP) |
Asymmetry(EP) |
1 |
impA |
4.668 |
6.452 |
42.1 |
1.49 |
12.54 |
14973 |
1.24 |
2 |
ER |
10.557 |
404.741 |
496.4 |
93.77 |
10.16 |
2864 |
4.91 |
3 |
impD |
17.203 |
12.065 |
47.6 |
2.80 |
2.77 |
17320 |
1.25 |
4 |
impE |
18.682 |
6.963 |
18.4 |
1.61 |
12.84 |
18749 |
1.14 |
5 |
ImpG |
27.308 |
1.408 |
2.5 |
0.33 |
N.a. |
18576 |
1.08 |
Sum |
431.628 |
|
100.00 |
38.31 |
|
|
Conclusion:
Welch column Ultisil XB-C8 (4.6×150mm, 3μm, 300A) was used to analyze the system suitability solution under this chromatographic condition. The retention time of the main peak was 10.6min, the separation between the main substance and the impurity was greater than 1.5, and the separation between impurity D and impurity E was greater than 2, which met the analysis requirements.