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Method for separating and determining rucotinib phosphate and impurities by high performance liquid chromatography

A technology of high performance liquid chromatography and alu phosphate, which is applied in the field of high performance liquid chromatography for separation and determination of ruxolitinib phosphate and impurities, and can solve the problem of inapplicability and influence on the content of active ingredients of the main drug, the production efficiency of pharmaceutical companies and the qualified rate of finished products. Adverse effects and other problems, to achieve the effect of strong specificity, good specificity and high accuracy

Active Publication Date: 2021-12-21
CHONGQING HUABANGSHENGKAI PHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are many impurities produced in the production process, which will inevitably affect the content of the active ingredients of the main drug, so the detection of impurities in the production process is particularly important
[0004] High performance liquid chromatography is often used in the detection of various drug impurities, but the chromatographic conditions for related substances in the import registration standard of ruxolitinib phosphate tablets (JX20140057) are not suitable for the detection of finished drugs of all manufacturers, and there is currently no simultaneous Specific methods for the separation and determination of the main drug and related impurities, which have a negative impact on the production efficiency and qualified rate of finished products of pharmaceutical companies

Method used

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  • Method for separating and determining rucotinib phosphate and impurities by high performance liquid chromatography
  • Method for separating and determining rucotinib phosphate and impurities by high performance liquid chromatography
  • Method for separating and determining rucotinib phosphate and impurities by high performance liquid chromatography

Examples

Experimental program
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Effect test

Embodiment 1

[0079] This embodiment specifically records the method for separating ruxolitinib phosphate and impurities by high performance liquid chromatography. The specific technical scheme is: mobile phase A is potassium dihydrogen phosphate, mobile phase B is methanol-acetonitrile; Silane-bonded silica gel;

[0080] Impurities include:

[0081] The method also separates the following impurities:

[0082]

[0083] Specifically, the elution ratio is:

[0084] 0min, the volume ratio of mobile phase A to mobile phase B is 70:30,

[0085] 2min, the volume ratio of mobile phase A to mobile phase B is 70:30,

[0086] 22min, the volume ratio of mobile phase A to mobile phase B is 48:52,

[0087] 27min, the volume ratio of mobile phase A to mobile phase B is 20:80,

[0088] 35min, the volume ratio of mobile phase A to mobile phase B is 20:80,

[0089] 36min, the volume ratio of mobile phase A to mobile phase B is 70:30,

[0090] 45min, the volume ratio of mobile phase A and mobile ...

Embodiment 2

[0100] On the basis of Example 1, this embodiment further illustrates the method for the determination of ruxolitinib phosphate and impurity content by high performance liquid chromatography, that is, the relevant condition parameters are specifically defined, as follows:

[0101] 1. Elution condition parameters

[0102] In this example, high performance liquid chromatography was used to separate and measure ruxolitinib phosphate and the content of impurities. The specific experimental conditions and parameters are shown in Table 2.

[0103] Table 2 High performance liquid chromatography separation and determination of ruxolitinib phosphate and impurity condition parameters

[0104]

[0105] 2. Solution preparation

[0106] Impurity B stock solution: Accurately weigh 25.56mg of the impurity B reference substance, put it in a 25ml measuring bottle, add acetonitrile to dissolve and dilute to the mark, shake well, and you get it.

[0107] Impurity C stock solution: Accuratel...

Embodiment 3

[0124] This example records other feasible chromatographic conditions, including elution gradient ratio, buffer salt type and concentration, flow rate, column temperature, etc.

[0125] 1. Research on different elution gradient ratios

[0126] Chromatographic column: Agilent ZORBAX SB-C18 4.6mm×250mm, 5μm

[0127] Column temperature: 25°C

[0128] Flow rate: 1.0ml / min

[0129] Mobile phase A: 0.03mol / L potassium dihydrogen phosphate aqueous solution (adjust pH to 3.5 with phosphoric acid)

[0130] Mobile Phase B: Methanol

[0131] Mobile Phase C: Acetonitrile

[0132] Elution gradient ratio 1: (HPLC picture as Figure 12 , the separation degree of each impurity meets the requirements)

[0133]

[0134]

[0135] Elution gradient ratio 2: (HPLC picture as Figure 13 , the separation degree of each impurity meets the requirements)

[0136] time (min) Mobile phase A(%) Mobile phase B(%) Mobile phase C(%) 0 70 15 15 2 70 15 15 20 60 ...

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Abstract

The invention relates to the field of analytical chemistry, and particularly discloses a method for separating and determining rucotinib phosphate and impurities by high performance liquid chromatography. According to the method, related chromatographic condition parameters are improved, so that the rucotinib phosphate and the impurities can be well separated, and qualitative and quantitative analysis is carried out on the main drug and the impurities thereof by utilizing the method. The method is good in specificity and is not interfered by a blank solvent and other unknown impurities, the separation degree between a main peak and the impurity B is 3.99, the separation degrees between other known impurities are all larger than 1.5, and the method has the advantages of being simple, rapid, high in accuracy and the like.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for separating and measuring ruxolitinib phosphate and impurities by high performance liquid chromatography. Background technique [0002] Ruxolitinib phosphate is a JAK1 / JAK2 inhibitor, which is mainly used for intermediate-risk or high-risk primary myelofibrosis (also known as chronic idiopathic myelofibrosis), myelofibrosis secondary to polycythemia vera Or adult patients with myelofibrosis secondary to essential thrombocythemia, for the treatment of disease-related splenomegaly or disease-related symptoms. [0003] The dose of ruxolitinib phosphate needs to be strictly controlled during the treatment process, and the platelet content in the patient's body should be periodically monitored, and the doctor will adjust the dose according to the relevant indicators. However, there are many impurities produced in the production process, which will inevitably affect the...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679G01N2030/065Y02P20/55
Inventor 李永玲杨婧侯立新余剑坤陈晨何国鑫杨飞
Owner CHONGQING HUABANGSHENGKAI PHARM
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