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| HPLC |
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| ≤ 0.5% | |
| SAL-A | ≤ 0.15% | |
SAL01-A | ≤ 0.15% | ||
SAL01-B | ≤ 0.3% | ||
| ≤ 0.10% | ||
| ≤ 1.0% | ||
| 98.0%~102.0% |
CAS号:2037-95-8 C 8 H NO 5 3 163.13
【Properties】Appearance This product should be white to brown light gray solid.
【Identification】In the chromatogram under the HPLC content determination item, the retention time of the main peak of the test solution was consistent with that of the reference solution.
【Inspection】
Moisture 0.2g of this product, precision weighing, anhydrous methanol as solvent, placed in a Karl Fischer titrator for determination.
related substances
Chromatographic conditions:
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| XTERRA RP18 4.6*250mm,5µm或等效柱 | |||||||||||||||||||||
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| 1.0ml/min | |||||||||||||||||||||
| 38min | |||||||||||||||||||||
| 210nm | |||||||||||||||||||||
| 25℃ | |||||||||||||||||||||
| 10µL | |||||||||||||||||||||
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Solution Preparation:
Diluent/blank: acetonitrile
Test solution: Weigh 20mg of the test sample accurately, put it in a 100ml measuring flask, add diluent to dissolve and dilute to the scale, and shake well.
Impurity mixed stock solution: 20mg of each SAL-A, SAL01-A, and SAL01-B reference substance was weighed in the same 100ml volumetric flask, dissolved with diluent and diluted to the scale, and shaken.
Resolution solution: 20mg of SAL01 reference substance was weighed accurately, placed in a 100ml measuring flask, 1ml of impurity mixed stock solution was added accurately, diluent was added to dissolve and diluted to the scale, and shaken well.
Control solution: 20mg of SAL01 reference substance was weighed accurately, placed in a 100ml measuring flask, dissolved with diluent and diluted to the scale, and shaken. Pipette 1.0ml accurately, put it in a 20ml measuring flask, dilute it to the scale with diluent, shake well, and then accurately pipette 1.0ml of the above solution, put it in a 50ml measuring flask, dilute it to the scale with diluent, and shake well.
Mensuration:
The blank solution, the resolution solution, the control solution, the self-control solution and the test solution were injected into the liquid chromatograph, the chromatogram was recorded, and the content of each impurity in the test sample was calculated according to the area normalization method. Impurities with a level of ˂0.025% were reported undetected.
System suitability requirements: The resolution of the main peak, known impurity peaks and adjacent peaks in the resolution solution is not less than 1.5. 6. The RSD of the irradiation solution shall not exceed 5%.
【Content】
Chromatographic conditions:
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| XTERRA RP18 4.6*250mm,5µm或等效柱 | |||||||||||||||||||||
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| 1.0ml/min | |||||||||||||||||||||
| 38min | |||||||||||||||||||||
| 210nm | |||||||||||||||||||||
| 25℃ | |||||||||||||||||||||
| 10µL | |||||||||||||||||||||
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Solution Preparation:
Diluent/blank solution: acetonitrile.
Reference solution: Weigh 10mg of SAL01 reference substance accurately, put it in a 100ml measuring flask, add diluent to dissolve and dilute to the scale, and shake well. Prepare 2 servings in parallel.
Test solution: Weigh 10mg of the test sample accurately, put it in a 100ml measuring flask, add diluent to dissolve and dilute to the scale, and shake well. Prepare 2 servings in parallel.
Mensuration:
The blank solution, the reference solution and the test solution were injected into the liquid chromatograph, and the control solution 1 was continuously injected with 6 needles, the control solution 2 was injected with 1 needle, and the test solution was injected with 1 needle each. The chromatogram was recorded, and the content of the test sample was calculated by the peak area according to the external standard method.
System applicability requirements: 6 For the retention time RSD of the main peak in solution 1 ≤1.0%, the ratio of the RF value (RF=peak area/concentration) of control solution 2 to the average RF value of control solution 1 is between 98%~102%.
File version revision history
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TS-SAL01-00-01 |
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