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HPLC (High-performance Liquid Chromatography) detecting method for febuxostat and related impurities thereof

A technology of febuxostat and a detection method, which is applied in the field of detection of 5 intermediate impurities of febuxostat, can solve the problems such as undiscovered 5 intermediate impurities of febuxostat, and achieves that it is not easily disturbed and has high precision. , the effect of improving stability

Active Publication Date: 2019-03-08
湖南新领航检测技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, in the current detection method, the control of the above-mentioned 5 intermediate impurities of febuxostat is carried out using different chromatographic conditions, and there is no literature report that can detect the 5 intermediate impurities of febuxostat at the same time.

Method used

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  • HPLC (High-performance Liquid Chromatography) detecting method for febuxostat and related impurities thereof
  • HPLC (High-performance Liquid Chromatography) detecting method for febuxostat and related impurities thereof
  • HPLC (High-performance Liquid Chromatography) detecting method for febuxostat and related impurities thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Embodiment 1: detection method of 5 intermediate impurities of febuxostat

[0054] 1) Chromatographic conditions

[0055] Instrument: Waters e2695+2489 high performance liquid chromatography;

[0056] Chromatographic column: C18, 250*4.6mm, 5um;

[0057] Column temperature: 30°C;

[0058] Flow rate of mobile phase: 1.0mL / min;

[0059] Detection wavelength: 215nm.

[0060] Trifluoroacetic acid solution: measure 1000ml of purified water and add 0.4ml of trifluoroacetic acid, mix well, and obtain;

[0061] Mobile Phase A: Trifluoroacetic acid solution

[0062] Mobile Phase B: Acetonitrile

[0063] Diluent: trifluoroacetic acid solution - acetonitrile (volume ratio 60:40)

[0064] Carry out gradient elution according to the following table 1;

[0065] Table 1: Conditions for gradient elution program

[0066] time (min)

Mobile phase A (v%)

Mobile phase B (v%)

0

40

60

8

40

60

30

30

70

35

30

70

35...

Embodiment 2

[0087] Embodiment 2: detection method of 5 intermediate impurities of febuxostat

[0088] Concretely carry out with reference to the detection method of embodiment 1, differs from embodiment 1 in that:

[0089] 1) The flow rate of the mobile phase is 1.2mL / min.

[0090] 2) Confirmation of impurities: the specific impurity names of the 5 intermediates of febuxostat are shown in Table 2

[0091] 3) Experimental results:

[0092] According to the positioning analysis of the five intermediate impurities of febuxostat, the five intermediate impurities of febuxostat and febuxostat can be determined, as shown in Table 2 in Example 1.

[0093] The 5 intermediate impurities and the main peak of febuxostat in the chromatogram were analyzed, and the results are shown in Table 4. The test results showed that the 5 intermediate impurities of febuxostat and febuxostat were well separated.

[0094] Table 4: Analysis results of impurities in the HPLC chromatograms of Example 2

[0095] ...

Embodiment 3

[0097] Embodiment 3: detection method of 5 intermediate impurities of febuxostat

[0098] Carry out with reference to the detection method of embodiment 1, difference with embodiment 1 is:

[0099] 1) Mobile phase:

[0100] Trifluoroacetic acid solution: Measure 1000ml of purified water and add 0.2ml of trifluoroacetic acid, mix well to obtain.

[0101] Mobile Phase A: Trifluoroacetic acid solution

[0102] Mobile Phase B: Acetonitrile

[0103] Diluent: trifluoroacetic acid solution-acetonitrile (60:40)

[0104] 2) Confirmation of impurities: the specific impurity names of the 5 intermediates of febuxostat are shown in Table 2

[0105] 3) Experimental results

[0106] According to the positioning analysis of the five intermediate impurities of febuxostat, the five intermediate impurities of febuxostat and febuxostat can be determined, as shown in Table 2 in Example 1.

[0107] The impurity peaks and main peaks in the chromatogram were analyzed, and the results are shown ...

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Abstract

The invention relates to the technical field of pharmaceutical analysis, in particular to a detecting method for febuxostat intermediate impurities. The detecting method adopts a high-performance liquid chromatography to perform determination, and comprises the following specific steps of: preparing a trifluoroacetic acid solution (a moving phase A), chromatographic-grade acetonitrile (a moving phase B), a diluent and a sample solution; and using a high-performance liquid chromatograph to detect the febuxostat in a prepared sample solution under the following conditions: a flow speed of 0.8 mL / min-1.2 mL / min, a column temperature of 30-40 DEG C, sample amount of 50 muL, a detecting wavelength of 215 nm, a chromatographic column of octadecylsilane bonded silica gel, a chromatographic columnelution program: the moving phase A:the moving phase B being 40:60 within 0-8 minutes, the moving phase A:the moving phase B being 40:60-30:70 within 8-30 minutes, the moving phase A:the moving phaseB being 30:70 within 30-35 minutes, and the moving phase A:the moving phase B being 30:70-40:60 within 35.1-40 minutes. The detecting method provided by the invention can effectively separate out five febuxostat intermediate impurities and the febuxostat.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a detection method for five intermediate impurities of febuxostat. Background technique [0002] Febuxostat is a new generation of non-purine selective xanthine oxidase inhibitors. It is a new drug for the treatment of gout. It has good curative effect and safety in the treatment of hyperuricemia and the gout caused by it. According to the existing febuxostat classic synthesis process, febuxostat undergoes 6 steps of reaction, and finally recrystallizes to obtain the finished product. During the synthesis process, a total of 5 intermediates are produced. Therefore, in order to obtain a qualified febuxostat bulk drug, the residue of febuxostat intermediate must be strictly and effectively controlled in the process of synthesizing the bulk drug, so as to avoid excessive unreacted intermediates from being brought into the bulk drug to form impurities. [0003] Febuxostat API ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 张瑜刘钊韦露思
Owner 湖南新领航检测技术有限公司