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A method for separating and determining degraded impurities in dutasteride raw materials and preparations by hplc method

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

Active Publication Date: 2021-06-01
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-ditrifluoromethylaniline is about 5 minutes, which is located in the middle of a large number of excipient peaks, with obvious interference , so the import standard is not applicable to the detection of this degraded impurity

Method used

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  • A method for separating and determining degraded impurities in dutasteride raw materials and preparations by hplc method
  • A method for separating and determining degraded impurities in dutasteride raw materials and preparations by hplc method
  • A method for separating and determining degraded impurities in dutasteride raw materials and preparations by hplc method

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Experimental program
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Effect test

Embodiment 1

[0035] Equipment and chromatographic conditions:

[0036] Japan Shimadzu SHIMADZULC-2010AHT liquid chromatograph; Detector: UV; Chromatographic column: octadecylsilane bonded silica gel is the chromatographic column (Kromasil 100-5C18, 250mm * 4.6mm, 5 μ m) of filler; With acetonitrile- Water-trifluoroacetic acid (520:480:0.25) was mobile phase A, methanol was mobile phase B, the flow rate was 1.0ml / min, the column temperature was 35°C, the detection wavelength was 310nm, and the injection volume was 50μl.

[0037] Gradient elution conditions:

[0038]

[0039] Detection steps:

[0040] 1. Preparation of the test solution: take 10 dutasteride soft capsules, pierce the top of the capsule with scissors, squeeze the contents into a 25ml measuring bottle, and use 70% acetonitrile aqueous solution to divide the scissors and the contents on the capsule shell After washing, the washing liquid was combined in the above-mentioned measuring bottle, diluted to the mark with 70% acet...

Embodiment 2

[0049] Embodiment 2 explores the conditions of the detection wavelength when detecting 2,5-bistrifluoromethylaniline.

[0050] Detection method:

[0051] Use octadecylsilane bonded silica gel as a chromatographic column (Kromasil 100-5C18, 250mm×4.6mm, 5μm, or a chromatographic column with equivalent performance); use acetonitrile-water-trifluoroacetic acid as mobile phase A, and use Methanol was the mobile phase B; the flow rate was 1ml / min; the column temperature was 35°C; the detection wavelengths were 220nm and 240nm.

[0052] Test results:

[0053] like figure 2 shown. According to the ultraviolet absorption spectrum, it is found that 2,5-bistrifluoromethylaniline has the maximum absorption near 240nm and 310nm. 240nm was used as the detection wavelength, and the blank excipients interfered with the detection. Therefore, the detection wavelength was initially selected as 310nm. In addition, compared with 220nm and 240nm, at 310nm wavelength, other known impurities a...

Embodiment 3

[0055] Embodiment 3 explores the conditions of diluent concentration when detecting 2,5-bistrifluoromethylaniline.

[0056] Detection method:

[0057] A chromatographic column (Kromasil 100-5C18, 250mm×4.6mm, 5μm, or a chromatographic column with equivalent performance) with octadecylsilane bonded silica gel as a filler, and acetonitrile-water-trifluoroacetic acid (520:480:0.25 ) is the mobile phase A, methanol is the mobile phase B; the flow rate is 1ml / min, the column temperature is 35°C, and the detection wavelength is 310nm.

[0058] Diluent: screen acetonitrile, 90% acetonitrile in water, 80% acetonitrile in water, 70% acetonitrile in water, 60% acetonitrile in water, 50% acetonitrile in water.

[0059] Detection steps: dilute the test sample with diluent solvents of different concentrations, and inject samples respectively according to the chromatographic method of the present invention.

[0060] Test results:

[0061] like image 3 shown. 1) Using 60% acetonitrile,...

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Abstract

The invention specifically relates to a method for separating and measuring degraded impurities in dutasteride raw materials and preparations by using high performance liquid chromatography, and the impurities are generated under forced degradation conditions. The method of the invention adopts octadecylsilane bonded silica gel as a chromatographic column, and uses mobile phase A and mobile phase B to carry out linear gradient elution. Since there are no quality standards for dutasteride soft capsules in the pharmacopoeias of various countries at present, and there are no relevant documents or standard reports, so this set of HPLC methods is a set of methods completely self-built. The present invention explores the detection wavelength, diluent Conditions such as mass concentration determine a set of methods suitable for the detection of the substance. The method has little interference during detection, has good specificity, good reproducibility and high accuracy, and can play a role in providing technical support for the quality control of dutasteride soft capsules.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring dutasteride raw materials and degraded impurities in preparations by using high performance liquid chromatography. Background technique [0002] Dutasteride is a white crystalline solid chemical with the formula C 27 h 30 F 6 N 2 O 2 , clinically mainly used for the treatment of enlarged prostate, male pattern hair loss, seborrheic alopecia and hereditary alopecia. The structural formula of dutasteride is as follows: [0003] [0004] 2,5-Ditrifluoromethylaniline is a degraded impurity produced by dutasteride soft capsules under strong acid, strong alkali 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: [0005] [0006] Upon inquiry, there is currently no quality standard for dutasteri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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