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Method for separating and determining degradation impurities in dutasteride raw material drug and preparation by virtue of HPLC

A technology of dutasteride and raw materials, applied in the field of analytical chemistry, can solve problems such as obvious interference, and achieve the effects of good specificity, high accuracy and good reproducibility

Active Publication Date: 2019-03-19
CHONGQING HUAPONT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the related substance method of the imported quality standard JX20130056, the relative retention time of the main component peak is about 6.5 minutes, and the peak time of the degraded impurity 2,5-ditr...

Method used

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  • Method for separating and determining degradation impurities in dutasteride raw material drug and preparation by virtue of HPLC
  • Method for separating and determining degradation impurities in dutasteride raw material drug and preparation by virtue of HPLC
  • Method for separating and determining degradation impurities in dutasteride raw material drug and preparation by virtue of HPLC

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Equipment and chromatographic conditions:

[0037] Shimadzu SHIMADZULC-2010AHT liquid chromatograph; detector: UV; chromatographic column: chromatographic column with octadecylsilane-bonded silica gel as filler (Kromasil 100-5C18, 250mm×4.6mm, 5μm); with acetonitrile- Water-trifluoroacetic acid (520:480:0.25) is the mobile phase A, methanol is the mobile phase B, the flow rate is 1.0ml / min, the column temperature is 35°C, the detection wavelength is 310nm; the injection volume is 50μl.

[0038] Gradient elution conditions:

[0039]

[0040] Detection steps:

[0041] 1. Preparation of test solution: Take 10 dutasteride soft capsules, pierce the top of the capsule with scissors, squeeze the contents into a 25ml measuring flask, and use 70% acetonitrile aqueous solution to divide the contents on the scissors and the capsule shell Wash the substance, combine the washing liquid in the above-mentioned measuring flask, add 70% acetonitrile aqueous solution to dilute to the mark, sh...

Embodiment 2

[0050] Example 2 is to explore the conditions of the detection wavelength when detecting 2,5-ditrifluoromethylaniline.

[0051] Detection method:

[0052] Chromatographic column with octadecylsilane-bonded silica gel as filler (Kromasil 100-5C18, 250mm×4.6mm, 5μm, or a column with equivalent performance); using acetonitrile-water-trifluoroacetic acid as mobile phase A, Methanol is the mobile phase B; the flow rate is 1ml / min; the column temperature is 35°C; the detection wavelength is 220nm and 240nm.

[0053] Test results:

[0054] Such as figure 2 Shown. According to the ultraviolet absorption spectrum, 2,5-ditrifluoromethylaniline has the maximum absorption at 240nm and 310nm. 240nm is used as the detection wavelength, and the blank auxiliary materials interfere with the detection. Therefore, the detection wavelength is initially selected as 310nm. In addition, compared with 220nm and 240nm, at 310nm wavelength, the response of other known impurities and blank excipients is l...

Embodiment 3

[0056] Example 3 is to explore the conditions of diluent concentration when detecting 2,5-ditrifluoromethylaniline.

[0057] Detection method:

[0058] Chromatographic column with octadecylsilane-bonded silica gel as filler (Kromasil 100-5C18, 250mm×4.6mm, 5μm, or equivalent column), with acetonitrile-water-trifluoroacetic acid (520:480:0.25) ) Is mobile phase A, methanol is used as mobile phase B; the flow rate is 1ml / min, the column temperature is 35°C, and the detection wavelength is 310nm.

[0059] Diluent: screening acetonitrile, 90% acetonitrile aqueous solution, 80% acetonitrile aqueous solution, 70% acetonitrile aqueous solution, 60% acetonitrile aqueous solution, 50% acetonitrile aqueous solution.

[0060] Detection step: Dilute the test product with diluent solvents of different concentrations, and separately sample for detection according to the chromatographic method of the present invention.

[0061] Test results:

[0062] Such as image 3 Shown. 1) Using 60% acetonitril...

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Abstract

The invention particularly relates to a method for separating and determining degradation impurities in a dutasteride raw material drug and a preparation by virtue of a high performance liquid chromatography. Impurities are generated under a forced degradation condition. According to the method, octadecylsilane bonded silica is taken as a chromatographic column for a filling agent, and linear gradient elution is carried out by virtue of a flow phase A and a flow phase B. Because a dutasteride soft capsule quality standard and any relevant literature or standard are not reported in pharmacopeias of each country, the HPLC is a set of a complete self-established method. By researching the conditions of detection wavelengths, diluent mass concentration and the like, a set of the method suitable for detecting the substance is determined and has the advantages that the detection interference is small, the specificity and the repeatability are good, the accuracy is high, and technical supportis provided for the mass control of a dutasteride soft capsule.

Description

Technical field [0001] The invention belongs to the field of analytical chemistry, and specifically relates to a method for separating and measuring dutasteride bulk drugs and degraded impurities in preparations by high performance liquid chromatography. Background technique [0002] Dutasteride is a white crystalline solid chemical with the molecular formula C 27 H 30 F 6 N 2 O 2 It is mainly used clinically to treat enlarged prostate, male pattern alopecia, seborrheic alopecia and hereditary alopecia. [0003] The structural formula of dutasteride is as follows: [0004] [0005] 2,5-Ditrifluoromethylaniline is a degradation impurity produced by dutasteride soft capsules under strong acid, strong base, and high temperature conditions. It is also the starting material for the synthesis of dutasteride. Its molecular formula is C 8 H 5 F 6 N, the structural formula is as follows: [0006] [0007] After inquiries, there is no quality standard for dutasteride soft capsules in the pharma...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/34G01N30/74G01N30/06
CPCG01N30/02G01N30/06G01N30/34G01N30/74
Inventor 张颖颜波
Owner CHONGQING HUAPONT PHARMA
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