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Shanghai Puyi Chemical Co., Ltd.

标准名称

卡沙兰(SAL01质量标准

标准编号

TS-SAL01-00-01

页码:

3/ 8

起草人/日期

审核人/日期

批准人/日期

生效日期:

20241015


Inspection items


Inspection standards


Characters


appearance


White to brownish light gray solid


Differential

HPLC


Under the content determination item, the retention time of the main peak of the test solution was consistent with that of the reference solution


examine


Moisture (KF)

0.5%


related substances

SAL-A

0.15%

SAL01-A

0.15%

SAL01-B

0.3%


Any unknown monomiscellaneous

0.10%


Total miscellaneous

1.0%


Content (as anhydrous)

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:


instrument


High performance liquid chromatograph


Detectors


Ultraviolet detector


Columns

XTERRA RP18 4.6*250mm5µm或等效柱


Mobile phase A


0.1% phosphoric acid in water


Mobile phase B


Acetonitrile


velocity of flow

1.0ml/min


Acquisition time

38min


Determine the wavelength

210nm


Column temperature

25℃


Injection volume

10µL


Gradient elution


Time

A%

B%

0

83

17

9

83

17

25

70

30

30

90

10

31

83

17

38

83

17


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:


instrument


High performance liquid chromatograph


Detectors


Ultraviolet detector


Columns

XTERRA RP18 4.6*250mm5µm或等效柱


Mobile phase A


0.1% phosphoric acid in water


Mobile phase B


Acetonitrile


velocity of flow

1.0ml/min


Acquisition time

38min


Determine the wavelength

210nm


Column temperature

25℃


Injection volume

10µL


Gradient elution


Time

A%

B%

0

83

17

9

83

17

25

70

30

30

90

10

31

83

17

38

83

17


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


Version number


Effective Date


Reasons for the revision and main contents

TS-SAL01-00-01


October 15, 2024


newly built