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Analysis and detection method of Palbociclib intermediates and their impurities

A technology for intermediates and impurities, applied in the field of pharmaceutical analytical chemistry, can solve problems such as reducing the solubility of drugs, and achieve the effect of effective control

Active Publication Date: 2018-05-15
北京元延医药科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Palbociclib is a yellow to orange powder that is a highly soluble compound at or below pH 4, but above pH 4 the drug is significantly less soluble

Method used

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  • Analysis and detection method of Palbociclib intermediates and their impurities
  • Analysis and detection method of Palbociclib intermediates and their impurities
  • Analysis and detection method of Palbociclib intermediates and their impurities

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0088] Instruments and conditions:

[0089] Shimadzu LC-2010AHT high performance liquid chromatograph and Shimadzu LC-solution workstation; Octadecylsilane bonded silica gel column (Waters C18, 4.6mm×150mm×5μm); use 0.01M ammonium acetate buffer as mobile phase A (unadjusted pH value is 6.6), acetonitrile as mobile phase B, perform linear gradient elution according to the elution gradient table above The detection wavelength is 235nm; the column temperature of the column oven is 30°C; the flow rate of the mobile phase is 1.0ml / min; the injection volume of the liquid phase analysis is 20μl.

[0090] experiment procedure:

[0091] Preparation of impurity stock solution: take appropriate amount of PB-SM1, PB-SM2, PB-1A, PB-1, PB-2D, PB-2B and PB-2A reference substances, weigh them accurately, add dichloromethane to dissolve and make A solution containing 0.2mg of PB-SM1, 0.2mg of PB-SM2, 0.2mg of PB-1A, 0.2mg of PB-1, 0.2mg of PB-2D, 0.2mg of PB-2B and 0.2mg of PB-2A in each 1...

Embodiment 2

[0098] Instruments and conditions:

[0099] Shimadzu LC-2010AHT high performance liquid chromatograph and Shimadzu LC-solution workstation; Octadecylsilane bonded silica gel column (Waters C18, 4.6mm×150mm×5μm); use 0.01M ammonium acetate buffer as mobile phase A, acetonitrile as mobile phase B, perform linear gradient elution according to the above table; detection wavelength is 235nm; column temperature is 30°C ; The flow rate of the mobile phase is 0.9ml / min; the injection volume of the liquid phase analysis is 20μl.

[0100] experiment procedure:

[0101] Preparation of impurity stock solution: take appropriate amount of PB-SM1, PB-SM2, PB-1A, PB-1, PB-2D, PB-2B and PB-2A reference substances, weigh them accurately, add dichloromethane to dissolve and make A solution containing 0.2mg of PB-SM1, 0.2mg of PB-SM2, 0.2mg of PB-1A, 0.2mg of PB-1, 0.2mg of PB-2D, 0.2mg of PB-2B and 0.2mg of PB-2A in each 1ml solution, as Impurity stock solution.

[0102] Preparation of syst...

Embodiment 3

[0107] Instruments and conditions:

[0108] Shimadzu LC-2010AHT high performance liquid chromatograph and Shimadzu LC-solution workstation; Octadecylsilane bonded silica gel column (Waters C18, 4.6mm×150mm×5μm); use 0.01M ammonium acetate buffer as mobile phase A, acetonitrile as mobile phase B, perform linear gradient elution according to the above table; detection wavelength is 235nm; column temperature is 30°C ; The flow rate of the mobile phase is 1.1ml / min; the injection volume of the liquid phase analysis is 20μl.

[0109] experiment procedure:

[0110] Preparation of impurity stock solution: take appropriate amount of PB-SM1, PB-SM2, PB-1A, PB-1, PB-2D, PB-2B and PB-2A reference substances, weigh them accurately, add dichloromethane to dissolve and make A solution containing 0.2mg of PB-SM1, 0.2mg of PB-SM2, 0.2mg of PB-1A, 0.2mg of PB-1, 0.2mg of PB-2D, 0.2mg of PB-2B and 0.2mg of PB-2A in each 1ml solution, as Impurity stock solution.

[0111] Preparation of syst...

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Abstract

The invention relates to an analysis and detection method of palbociclib intermediates and impurities in the palbociclib intermediates, in particular to a mass analysis method of the palbociclib intermediates. The method comprises the step of conducting mass analysis on the palbociclib intermediates by the adoption of an efficient liquid chromatography. According to the method, an adopted chromatographic column is a chromatographic column C18, and the column temperature is 28-45 DEG C. According to the method, by the adoption of the liquid chromatography, the palbociclib intermediates and the impurities in the palbociclib intermediates are effectively separated under certain chromatographic conditions, and the content of the impurities in the palbociclib intermediates can be accurately determined by the method.

Description

technical field [0001] The invention belongs to the field of pharmaceutical analytical chemistry, and relates to a method for analyzing the quality of an intermediate of the antineoplastic drug palbociclib, in particular to the separation and determination of the intermediate of palbociclib and its Analytical methods for relevant impurities. Background technique [0002] Palbociclib is an inhibitor of cyclin-dependent kinase (CDK) 4 and CDK6. Cyclin D1 and CDK4 / 6 are downstream of signaling pathways leading to cell proliferation. In vitro, palbociclib reduces cell proliferation in estrogen receptor (ER)-positive breast cancer cell lines by blocking cell cycle progression from G1 to S phase. Co-administration of palbociclib and an anti-estrogen reduces retinoblastoma protein (Rb) phosphorylation leading to E2F expression and prevents increased growth compared with each drug alone. In vitro treatment of ER-positive breast cancer cell lines with the combination of palbocicli...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/89
CPCG01N30/89
Inventor 甘兴杰王立强
Owner 北京元延医药科技股份有限公司