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HPLC analysis method of mirabegron-related substances

An analysis method and related substance technology, applied in the field of drug analysis of aryl ethanolamine β3 receptor agonists, can solve the problems of incomplete detection and interference of impurity detection, and achieve fast analysis speed, reliable impurity control, and good accuracy

Active Publication Date: 2020-02-21
ZHEJIANG HUAYI PHARMA CO LTD OF HANGZHOU HUADONG PHARMA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above methods all detect the impurities existing in the Mirabegron API, the detection is not comprehensive, and the above methods all use ion-pairing reagents as eluents, which easily interfere with the detection of impurities

Method used

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  • HPLC analysis method of mirabegron-related substances
  • HPLC analysis method of mirabegron-related substances
  • HPLC analysis method of mirabegron-related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Detection method:

[0054]Take an appropriate amount of Mirabegron test sample, weigh it accurately, add 30% methanol to dissolve and dilute it into a sample solution of 1 mg / ml, shake it up, and accurately measure 20 μl and inject it into the liquid chromatograph. Perform HPLC analysis at 30°C and record the chromatograms.

[0055] The concentration of potassium dihydrogen phosphate buffer in mobile phase A is 0.02mol / L, the pH is 5.5, and the ratio of methanol is 12%.

[0056] Analyze the system suitability solution according to the following gradient elution procedure

[0057] time (min) Mobile phase A% Mobile phase B% 0 100 0 5 100 0 40 50 50 50 50 50 51 100 0 60 100 0

[0058] Chromatogram see figure 1 , the retention time of each impurity and the main peak and the resolution between adjacent peaks are shown in Table 1.

[0059] Table 1

[0060]

[0061]

[0062] From the data in Table 1, it can be se...

Embodiment 2

[0064] Others are the same as embodiment 1, the difference is:

[0065] The concentration of potassium dihydrogen phosphate buffer in mobile phase A is 0.01mol / L or 0.05mol / L;

[0066] Analyze the system adaptability solution according to the gradient elution program in Example 1, see the chromatogram figure 2 with 3 , the retention time of each impurity and the main peak and the resolution between adjacent peaks are shown in Table 2 and Table 3.

[0067] When the concentration of potassium dihydrogen phosphate buffer solution in mobile phase A in table 2 is 0.01mol / L, the result of resolution

[0068]

[0069]

[0070] When the concentration of potassium dihydrogen phosphate buffer solution in mobile phase A in table 3 is 0.05mol / L, the result of resolution

[0071] name / code retention time (min) Resolution between adjacent peaks Impurity A 3.187 / Impurity B 15.583 42.14 Impurity C 21.152 34.26 Mirabegron 24.182 11.40 ...

Embodiment 3

[0075] Others are the same as embodiment 1, the difference is:

[0076] The pH of potassium dihydrogen phosphate buffer in mobile phase A is 4.0 or 6.5;

[0077] Analyze the system adaptability solution according to the gradient elution program in Example 1, see the chromatogram Figure 4 with 5 , the retention time of each impurity and the main peak and the resolution between adjacent peaks are shown in Table 4 and Table 5.

[0078] The separation result when the pH of potassium dihydrogen phosphate buffer in table 4 mobile phase A is 4.0

[0079]

[0080]

[0081] The separation result when the pH of potassium dihydrogen phosphate buffer solution in table 5 mobile phase A is 6.5

[0082] name / code retention time (min) Resolution between adjacent peaks Impurity A 3.243 / Impurity B 15.281 39.99 Impurity C 21.927 40.61 Mirabegron 25.165 12.15 Impurity D 27.470 5.85 Impurity E 28.953 3.92 Impurity F 31.375 ...

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Abstract

The invention discloses an HPLC analysis method of mirabegron-related substances. The HPLC analysis method includes the steps that octadecyl silane chemically bonded silica is selected to be taken asa chromatographic column of a filler; a mobile phase is adopted for carrying out gradient elution, and the mobile phase is prepared from the compositions of a potassium dihydrogen phosphate buffer solution, methanol and acetonitrile; and high performance liquid chromatograph is carried out at appropriate velocity and column temperature, and a chromatogram is recorded. Impurities in a mirabegron raw material drug can be effectively eluted, separated and quantified, an impurity peak is completely separated from a main peak, the analysis speed is fast, and the detection effect is good.

Description

technical field [0001] The invention belongs to the technical field of aryl ethanolamine β3 receptor agonist drug analysis, and in particular relates to an HPLC analysis method for mirabegron related substances. Background technique [0002] Mirabegron ((R)-2-(2-amino-1,3-thiazol-4-yl)-4'-[2-[(2-hydroxy-2-phenylethyl)amino]ethyl] Phenylacetamide) belongs to the aryl ethanolamine β3 receptor agonist, acts on the β3 adrenergic receptor of the detrusor smooth muscle of the bladder, dilates the bladder, promotes bladder filling and increases urine storage, can effectively reduce the frequency of urination, and improve bladder overactivity. urinary frequency, urgency and urinary incontinence. Mirabegron provides a new treatment plan for patients with overactive bladder. Its tablet is convenient to take, the dosage is small, and the drug effect is significant. It can significantly relieve the pain of patients with overactive bladder and bring good news to the majority of patients...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/34G01N30/86
CPCG01N30/8679G01N30/02G01N30/34
Inventor 陈向明朱书剑楼金萍陈方琴杜子为
Owner ZHEJIANG HUAYI PHARMA CO LTD OF HANGZHOU HUADONG PHARMA GRP
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