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Method for determining dapagliflozin and its related substance by high performance liquid chromatograph

A technology of high performance liquid chromatography and related substances, which is applied in the field of high performance liquid chromatography for the determination of dapagliflozin and its related substances, can solve the problems that have not been seen about the detection methods of related substances of dapagliflozin, and achieve strong specificity , easy operation and high precision

Active Publication Date: 2017-12-26
湖北石河医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there is no detection method for related substances of dapagliflozin

Method used

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  • Method for determining dapagliflozin and its related substance by high performance liquid chromatograph
  • Method for determining dapagliflozin and its related substance by high performance liquid chromatograph
  • Method for determining dapagliflozin and its related substance by high performance liquid chromatograph

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Chromatographic column: Agilent Eclipse XDB-C18 (250*4.6mm, 5μm);

[0061] Mobile phase A: 0.01% phosphoric acid aqueous solution;

[0062] Mobile phase B: acetonitrile;

[0063] Gradient elution conditions:

[0064]

[0065]

[0066] Column temperature: 30°C;

[0067] Detection wavelength: 224nm;

[0068] Flow rate: 1.0mL / min;

[0069] Injection volume: 10μL;

[0070] Running time: 70min;

[0071] Experimental steps:

[0072] Diluent: acetonitrile-water (80:20) (v / v)

[0073] Blank solution: diluent

[0074] Impurity control stock solution: take about 10 mg each of the impurity A reference substance, impurity B reference substance, and impurity C reference substance, weigh them accurately, put them in the same 100ml volumetric flask, dissolve them with diluent and dilute to the mark, shake well, and have to.

[0075] Darpagliflozin reference substance stock solution: Take about 20 mg of Dapagliflozin reference substance, accurately weigh it, put it in a...

Embodiment 2

[0085] Chromatographic column: Agilent Eclipse XDB-C18 (250*4.6mm, 5μm);

[0086] Mobile phase A: 0.01% phosphoric acid aqueous solution;

[0087] Mobile phase B: Methanol;

[0088] Gradient elution conditions:

[0089] time (minutes)

Mobile phase A (V%)

Mobile phase B (V%)

0

72

28

30

55

45

45

20

80

55

5

95

60

5

95

60.1

72

28

70

72

28

[0090] Column temperature: 35°C;

[0091] Detection wavelength: 224nm;

[0092] Flow rate: 1.2mL / min;

[0093] Injection volume: 10μL;

[0094] Running time: 70min;

[0095] Experimental steps:

[0096] Diluent: acetonitrile-water (80:20) (v / v);

[0097] Blank solution: diluent;

[0098] Impurity control stock solution: take about 10 mg each of the impurity A reference substance, impurity B reference substance, and impurity C reference substance, weigh them accurately, put them in the same 100ml volumetric flask, dissolve them with...

Embodiment 3

[0109] Chromatographic column: Agilent Eclipse XDB-C18 (250*4.6mm, 5μm);

[0110] Mobile phase A: 0.01% phosphoric acid aqueous solution;

[0111] Mobile phase B: acetonitrile;

[0112] Gradient elution conditions:

[0113] time (minutes)

Mobile phase A(%)

Mobile phase B(%)

0

68

32

30

55

45

45

10

90

55

5

95

60

5

95

60.1

68

32

70

68

32

[0114] Column temperature: 25°C;

[0115] Detection wavelength: 224nm;

[0116] Flow rate: 0.8mL / min;

[0117] Injection volume: 10μL;

[0118] Running time: 70min;

[0119] Experimental steps:

[0120] Diluent: acetonitrile-water (80:20) (v / v)

[0121] Blank solution: diluent

[0122] Impurity control stock solution: take about 10 mg each of the impurity A reference substance, impurity B reference substance, and impurity C reference substance, weigh them accurately, put them in the same 100ml volumetric flask, dissolve them with d...

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Abstract

The invention discloses a method for determining dapagliflozin and its related substance by a high performance liquid chromatograph. The high performance liquid chromatography utilizes an octadecylsilane bonded silica gel column as a chromatographic column, an acidic aqueous solution as a mobile phase A and a first organic solvent as a mobile phase B for gradient elution. The method has high sensitivity, high specificity, high precision, high accuracy, simple and quick operation and wide applicability range, realizes separation and determination of the dapagliflozin bulk drug and related substances of a dapagliflozin preparation under the same chromatographic conditions and effectively controls the quality of drugs.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis. Specifically, the invention relates to a method for measuring dapagliflozin and its related substances by using a high performance liquid chromatography. Background technique [0002] Dapagliflozin (Farxiga, compound shown in formula 1), developed by Bristol Myers Squibb, is a type 2 sodium ion-dependent glucose cotransporter (sodium-dependent glucosecotransporter 2, SGLT2) inhibitor, released on January 2014 It was approved by the FDA for the treatment of type 2 diabetes on August 8. [0003] [0004] During the preparation process of Daxigliflozin, multiple impurities may be produced due to various factors such as raw materials, synthesis process, and degradation. Among them, impurity A, impurity B and impurity C are the three impurities that are difficult to control in the synthesis process. The researchers set these three impurities as the specific impurities of Daxigliflozin pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/88G01N30/34
CPCG01N30/02G01N30/34G01N30/88G01N2030/884G01N2030/027
Inventor 徐先英祝小芬钱丽娜
Owner 湖北石河医药科技有限公司
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