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Method for separating and determining baricitinib bulk drug impurities by using HPLC

A technology for raw materials and impurities, which is applied in the field of analysis and determination of baricitinib raw materials, can solve the problems of lack of rapid, simple and accurate analysis and detection of baricitinib raw materials, and achieves high sensitivity and high precision. , the effect of strong accuracy

Active Publication Date: 2020-11-27
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

[0006] In order to control the quality of baricitinib 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 related substances of baricitinib API

Method used

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  • Method for separating and determining baricitinib bulk drug impurities by using HPLC
  • Method for separating and determining baricitinib bulk drug impurities by using HPLC
  • Method for separating and determining baricitinib bulk drug impurities by using HPLC

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Chromatographic column: ChromCore C18(2)5μm250×4.6mm

[0059] Mobile phase A: water

[0060] Mobile Phase B: Acetonitrile

[0061] Column temperature: 35℃

[0062] Flow rate: 1.0ml / min

[0063] Detection wavelength: 224nm

[0064] Injection volume: 10μl

[0065] The conditions of gradient elution are:

[0066] Time, minutes Mobile phase A, volume% Mobile phase B, volume% 09010 39010 452080 469010 559010

[0067] Sample preparation:

[0068] Thinner: Acetonitrile

[0069] Blank solution: thinner

[0070] Reference substance solution: Take about 20mg of Baritinib working reference substance, accurately weigh it, place it in a 20ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, accurately measure 1ml to 10ml, add diluent to dissolve and dilute To the mark, shake well, and then accurately measure 1ml to 10ml, add diluent to dissolve and dilute to the mark, shake, and then accurately measure 1ml to 10ml, add the diluent to dissolve and dilute to the mark, ...

Embodiment 2

[0086] Chromatographic column: ChromCoreC18(2)5μm250×4.6mm

[0087] Mobile phase A: water

[0088] Mobile Phase B: Acetonitrile

[0089] Column temperature: 35℃

[0090] Flow rate: 1.0ml / min

[0091] Detection wavelength: 224nm

[0092] Injection volume: 10μl

[0093] The conditions of gradient elution are:

[0094] Time, minutes Mobile phase A, volume% Mobile phase B, volume% 0905 3905 452080 46905 55905

[0095] Sample preparation:

[0096] The same sample preparation as in Example 1.

[0097] Take the above solutions separately, perform high performance liquid chromatography analysis under the above chromatographic conditions, record the chromatograms, and see the results Figure 7 , Attached Figure 8 , Attached Picture 9 , Attached Picture 10 , Attached Picture 11 , Attached Picture 12 .

[0098] in conclusion: Figure 7 Indicates that the blank does not interfere with the impurity inspection; Figure 8 It shows that the detection limits of baritinib and impurity A, impurity B, im...

Embodiment 3

[0102] Chromatographic column: ChromCoreC18(2)5μm250×4.6mm

[0103] Mobile phase A: water

[0104] Mobile Phase B: Acetonitrile

[0105] Column temperature: 35℃

[0106] Flow rate: 1.0ml / min

[0107] Detection wavelength: 224nm

[0108] Injection volume: 10μl

[0109] The conditions of gradient elution are:

[0110] Time, minutes Mobile phase A, volume% Mobile phase B, volume% 09010 39010 452575 469010 559010

[0111] Sample preparation:

[0112] The same sample preparation as in Example 1.

[0113] Take the above solutions separately, perform high performance liquid chromatography analysis under the above chromatographic conditions, record the chromatograms, and see the results Figure 13 , Attached Figure 14 , Attached Figure 15 , Attached Figure 16 , Attached Figure 17 , Attached Figure 18 .

[0114] in conclusion: Figure 13 Indicates that the blank does not interfere with the impurity inspection; Figure 14 It shows that the detection limits of baritinib and impurity A, impurity...

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Abstract

The invention relates to a method for separating and determining impurities in a baricitinib bulk drug by using HPLC (High Performance Liquid Chromatography). The method comprises the following steps:step 1, taking a baricitinib bulk drug sample, carrying out gradient elution by using octadecylsilane chemically bonded silica as a filler, water as a mobile phase A and acetonitrile as a mobile phase B, and taking eluent as a detection sample; step 2, performing preparation of a detection liquid: taking a baricitinib bulk drug detection sample, a baricitinib reference substance, an impurity A, an impurity B, an impurity C, an impurity D and an impurity E, and preparing a high performance liquid chromatography analysis liquid; and step 3, carrying out high performance liquid chromatography analysis on the detection liquid prepared in the step 2; obtaining the content of each impurity. According to the method, the comprehensive influence of an analysis column, a mobile phase, a gradient elution program, a flow rate and a column temperature on separation detection is comprehensively considered, so that a detection result is optimized; and the method has the advantages of rapidness, simplicity, convenience, high sensitivity, accuracy, reliability and wide applicability, and is suitable for separating and determining the impurity content of the baricitinib bulk drug.

Description

Technical field [0001] The invention relates to an analysis and determination method of baritinib bulk medicine, in particular to a method for separating and determining impurities of baritinib bulk medicine by HPLC. Background technique [0002] Baricitinib, a selective oral Janus kinase-1 (JAK1) and JKA2 inhibitor jointly developed by Eli Lilly and Incyte Pharmaceuticals, can inhibit interleukin-6 (IL-6) and leukocytes Intracellular signal transduction of various inflammatory cytokines such as interleukin-23 (IL-23). In 2017, it was approved for marketing by the European Union and approved by the FDA in 2018. New research has found that baritinib may prevent the infection process of the new coronavirus in 2019 and predicts that it can reduce the ability of this virus to infect lung cells. [0003] The molecular formula is C 16 H 17 N 7 O 2 S, the molecular weight is 371.42, and the structural formula is as follows: [0004] [0005] During the preparation of Baritinib, many impur...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/36G01N30/60G01N30/74
CPCG01N30/02G01N30/06G01N30/34G01N30/36G01N30/74G01N30/60
Inventor 吴其华葛德培陈海兵李强邵广晴
Owner 安徽联创生物医药股份有限公司
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