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A kind of method for separating and measuring impurities of baricitinib bulk drug by 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 the effect of high sensitivity

Active Publication Date: 2022-07-01
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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  • A kind of method for separating and measuring impurities of baricitinib bulk drug by hplc
  • A kind of method for separating and measuring impurities of baricitinib bulk drug by hplc
  • A kind of method for separating and measuring impurities of baricitinib bulk drug by 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 for gradient elution are:

[0066] time, minutes Mobile phase A, vol% Mobile phase B, vol% 0 90 10 3 90 10 45 20 80 46 90 10 55 90 10

[0067] Sample preparation:

[0068] Thinner: Acetonitrile

[0069] Blank solution: diluent

[0070] Reference substance solution: take about 20 mg of baricitinib working reference substance, accurately weigh it, put 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, then accurately measure 1ml to 10ml, add a diluent to dissolve and dilute to the mark, shake well, then accurately m...

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 for gradient elution are:

[0094] time, minutes Mobile phase A, vol% Mobile phase B, vol% 0 90 5 3 90 5 45 20 80 46 90 5 55 90 5

[0095] Sample preparation:

[0096] Prepared with the sample in Example 1.

[0097] Get above-mentioned solution respectively, carry out high-performance liquid chromatographic analysis in above-mentioned chromatographic condition, record chromatogram, the result is shown in the attached Figure 7 , attached Figure 8 , attached Figure 9 , attached Figure 10 , attached Figure 11 , attached Figure 12 .

[0098] in conclusion: Figure 7 Indicates that the blank does not interfere with the impurity check; ...

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 for gradient elution are:

[0110] time, minutes Mobile phase A, vol% Mobile phase B, vol% 0 90 10 3 90 10 45 25 75 46 90 10 55 90 10

[0111] Sample preparation:

[0112] Prepared with the sample in Example 1.

[0113] Get above-mentioned solution respectively, carry out high-performance liquid chromatographic analysis in above-mentioned chromatographic condition, record chromatogram, the result is shown in the attached 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...

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Abstract

The invention relates to a method for separating and measuring impurities of a baricitinib bulk drug by HPLC, comprising the following steps: Step 1, taking a baricitinib bulk drug sample, using octadecylsilane-bonded silica gel as a filler, and adding water Carry out gradient elution with mobile phase A and acetonitrile as mobile phase B, and take the eluent as the detection sample; step 2, prepare the detection solution, and take the baricitinib API test sample, baricitinib reference substance, and impurity A , impurity B, impurity C, impurity D, impurity E, prepare high performance liquid chromatography analysis liquid; Step 3, carry out high performance liquid chromatography analysis to the detection liquid prepared in step 2; Obtain the content of each impurity; The comprehensive effects of analytical column, mobile phase, gradient elution procedure, flow rate and column temperature on separation and detection have optimized the detection results. It has the advantages of rapidity, simplicity, high sensitivity, accuracy and reliability, and wide applicability. It is suitable for separation and determination. Impurity content of baricitinib drug substance.

Description

technical field [0001] The present invention relates to a method for analyzing and measuring baricitinib crude drug, in particular to a method for separating and measuring impurities of baricitinib crude drug by HPLC. Background technique [0002] Baricitinib, a selective oral Janus kinase-1 (JAK1) and JKA2 inhibitor jointly developed by Eli Lilly and Company and Incyte Pharmaceuticals, can inhibit interleukin-6 (IL-6) and white blood cells Intracellular signaling of various inflammatory cytokines such as interferon-23 (IL-23). In 2017, it was approved for marketing by the European Union and in 2018 by the FDA. New research found that baricitinib may prevent the infection process of the 2019 novel coronavirus and predict that it can reduce the ability of the 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 baricitini...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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