Method for separating and measuring dapagliflozin crude drug related substance through HPLC

A technology related to substances and raw materials, applied in the field of analytical chemistry, can solve the problems of no fast, simple and accurate analysis and detection of Dapagliflozin raw materials, and achieve the effect of accurate and reliable operation, high sensitivity and strong specificity

Active Publication Date: 2019-02-22
安徽联创生物医药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0023] In order to control the quality of Dapagliflozin API, it is necessary to control the main components and impurities. In the existing technology, there is no analytical method suitable for fast, simple and accurate analysis and detection of Dapagliflozin API related substances

Method used

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  • Method for separating and measuring dapagliflozin crude drug related substance through HPLC
  • Method for separating and measuring dapagliflozin crude drug related substance through HPLC
  • Method for separating and measuring dapagliflozin crude drug related substance through HPLC

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Chromatographic conditions:

[0050] Chromatographic column: Agilent 5TC-C18(2) 250×4.6mm

[0051] Mobile Phase A: Water

[0052] Mobile Phase B: Acetonitrile

[0053] Column temperature: 30°C

[0054] Flow rate: 1.0ml / min

[0055] Detection wavelength: 224nm

[0056] Injection volume: 20μl

[0057] The gradient elution program is:

[0058] Table 1 Gradient elution program

[0059] time, minutes

Mobile phase A, volume %

Mobile phase B, volume %

0

72

28

10

72

28

40

10

90

55

10

90

56

72

28

70

72

28

[0060] Solution preparation:

[0061] Impurity reference substance stock solution: take impurity A reference substance, impurity B reference substance, impurity C reference substance, impurity D reference substance, impurity E reference substance, impurity F reference substance, impurity G reference substance, impurity H reference substance, impurity I control substance About ...

Embodiment 2

[0071] Chromatographic conditions:

[0072] Chromatographic column: Agilent 5TC-C18(2) 250×4.6mm

[0073] Mobile Phase A: Water

[0074] Mobile Phase B: Acetonitrile

[0075] Column temperature: 30°C

[0076] Flow rate: 1.0ml / min

[0077] Detection wavelength: 224nm

[0078] Injection volume: 20μl

[0079] The gradient elution program is:

[0080] Table 3 Gradient elution program

[0081] time, minutes

Mobile phase A, volume %

Mobile phase B, volume %

0

72

26

10

72

26

43

10

90

55

10

90

56

72

26

70

72

26

[0082] Solution preparation:

[0083] Impurity reference substance stock solution: take impurity A reference substance, impurity B reference substance, impurity C reference substance, impurity D reference substance, impurity E reference substance, impurity F reference substance, impurity G reference substance, impurity H reference substance, impurity I control substance Abou...

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Abstract

The invention provides a method for separating and measuring dapagliflozin crude drug related substance through a HPLC. The method comprises the following steps: performing gradient elution by takingoctadecylsilane chemically bonded silica as a filler, water as a flowing phase A and acetonitrile as a flowing phase B, ensuring that the flow rate is 0.8 to 1.2ml/min and the column temperature is 25to 40 DEG C, adopting an ultraviolet detector to detect the dapagliflozin crude drug related substance, and ensuring that the detection wavelength of the ultraviolet detector is 205 to 230nm. The method ensures that detection results are optimized through overall consideration of comprehensive influence on separation and detection by an analytical column, flowing phases, a gradient elution program, the flow rate and the column temperature, thereby effectively controlling the quality of crude drugs. In addition, the method has the advantages of high rapidness, simpleness, sensitivity, specificity, precision, accuracy, reliability and convenience in operation, and is applied to separation and measurement of the dapagliflozin crude drug related substance.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a method for separating and measuring related substances of dapagliflozin bulk drug by HPLC. Background technique [0002] Dapagliflozin (trade name Farxiga), a new type of anti-diabetic drug jointly developed by Bristol-Myers Squibb and AstraZeneca, was approved for marketing by the European Medicines Agency on November 12, 2012. A SGLT2 inhibitor approved for the treatment of type 2 diabetes. On January 8, 2014, it was approved by the US FDA for marketing to improve blood sugar control in adults with type 2 diabetes. Dapagliflozin is a new sodium-glucose cotransporter 2 (SGLT2) inhibitor drug, which can reduce the elevated blood sugar level in diabetic patients by inhibiting the reabsorption of glucose by the kidney and increasing glucose excretion. Molecular formula is C 21 h 25 ClO 6 ·C 3 h 8 o 2 ·H 2 O, the molecular weight is 502.98, and the structural...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 吴其华葛德培陈海兵
Owner 安徽联创生物医药股份有限公司
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