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Method for separation and determination of Palbociclib intermediate Z1 and related substances

A technology related to substances and intermediates, applied in the field of analytical chemistry, to achieve the effect of strong specificity and high sensitivity

Inactive Publication Date: 2018-01-05
CHONGQING HUABANGSHENGKAI PHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, in order to control the quality of palbociclib intermediate Z1, it is particularly important to separate and measure palbociclib intermediate Z1 and its related substances. At present, there is no published method to report the separation and determination of palbociclib intermediate Method for body Z1 and its related substances

Method used

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  • Method for separation and determination of Palbociclib intermediate Z1 and related substances
  • Method for separation and determination of Palbociclib intermediate Z1 and related substances
  • Method for separation and determination of Palbociclib intermediate Z1 and related substances

Examples

Experimental program
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Effect test

Embodiment 1

[0099] Example 1 Method for separating and determining palbociclib intermediate Z1 and related substances by high performance liquid chromatography

[0100] (1) Prepare blank solution (diluent): take 25ml of 0.1% trifluoroacetic acid aqueous solution, put it in a 100ml measuring bottle, add acetonitrile to dilute to the mark, shake well, and you get it;

[0101] (2) Prepare impurity localization solution: take palbociclib intermediate Z1 impurity reference substance, dissolve and dilute with diluent to obtain impurity localization solution;

[0102] (3) Preparation of the test solution: get about 25 mg of palbociclib intermediate Z1, accurately weighed, put in a 50ml measuring bottle, add diluent to dissolve and dilute to the scale, shake up, as the test solution;

[0103] (4) Prepare self-contrast solution: accurately pipette 1.0ml of the test solution, put it in a 100ml measuring bottle, add diluent to dilute to the mark, shake well, and get final product;

[0104] (5) Prep...

Embodiment 2

[0106] Example 2 The separation degree of palbociclib intermediate Z1 and its related substances by the high performance liquid chromatography system of the present invention

[0107] (1) Prepare blank solution (diluent): take 25ml of 0.1% trifluoroacetic acid aqueous solution, put it in a 100ml measuring bottle, add acetonitrile to dilute to the mark, shake well, and you get it;

[0108] (2) Preparation of the test solution: Accurately weigh 26.63mg of intermediate Z1, put it in a 50ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and then get the test solution with a concentration of 0.5326mg / ml ;

[0109] (3) Preparation of impurity positioning solution:

[0110] Impurity 1 stock solution: Accurately weigh 13.83mg of impurity 1, put it in a 25ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and the concentration is 553.2μg / ml;

[0111] Impurity 2 stock solution: Accurately weigh 11.32mg of impurity 2, put it ...

Embodiment 3

[0116] Example 3 The detection level of palbociclib intermediate Z1 and its related substances by the high performance liquid chromatography system of the present invention

[0117] (1) Prepare blank solution (diluent): take 25ml of 0.1% trifluoroacetic acid aqueous solution, put it in a 100ml measuring bottle, add acetonitrile to dilute to the mark, shake well, and you get it;

[0118] (2) Prepare the test solution: accurately weigh 26.63mg of intermediate Z1, put it in a 50ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and the concentration is 0.5326mg / ml;

[0119] (3) Prepare self-contrast solution: accurately pipette 1.0ml of the test solution, put it in a 100ml measuring bottle, add diluent to dilute to the mark, shake well, and get final product;

[0120] (4) Prepare secondary dilution of intermediate Z1: accurately pipette 1.0ml of self-contrast solution, put it in a 10ml measuring bottle, add diluent to dilute to the mark, shake well, ...

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Abstract

Belonging to the field of analytical chemistry, the invention in particular relates to a method for separation and determination of a Palbociclib intermediate Z1 and related substances. The method takes octadecyl silane bonded silica gel as the stationary phase, and employs the mixed liquid of water and an organic solvent as the mobile phase for elution, wherein the organic solvent is one or moreof methanol, acetonitrile, ethanol and isopropyl alcohol. The method also can completely separate the Palbociclib intermediate Z1 and related substances, during detection, the solvent peak does not interfere with the determination of Palbociclib intermediate Z1 and related substances, and the separation degree is greater than 1.5. The method has the advantages of strong specificity, good stabilityand high sensitivity, can effectively separate the Palbociclib intermediate Z1 and related substances, and is of very important significance for quality control and safety guarantee of the Palbociclib intermediate Z1.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring palbociclib intermediate Z1 and its related substances. Background technique [0002] Palbociclib, trade name IBRANCE, is the first FDA-approved cyclin-dependent kinase 4 / 6 (CDKs4 / 6) inhibitor. CDKs4 and 6, as key regulators of the cell cycle, can trigger cell cycle progression. The indication of IBRANCE in the United States is combined with letrozole for the treatment of estrogen receptor positive, human epidermal growth factor receptor 2 negative (ER+ / HER2-) postmenopausal patients with advanced breast cancer, as an initial endocrine therapy-based regimen Treatment of metastatic disease. Palbociclib intermediate Z1 is a key intermediate for the synthesis of palbociclib, and its molecular formula is C 27 h 34 BrN 7 o 3 , molecular weight 584.52, intermediate Z1 chemical name: tert-Butyl 4-[6-(6-bromo-8-cyclopentyl-5-methy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 李江玲唐舒棠
Owner CHONGQING HUABANGSHENGKAI PHARM
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