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HPLC analysis method for estrone-related substances

An analysis method and technology of related substances, applied in the field of HPLC analysis of related substances of estrone, can solve the problems of inaccurate quantification of impurity C, impurity F cannot be eluted, and cannot be effectively separated, achieving accurate determination and fast analysis speed Effect

Active Publication Date: 2018-08-24
ZHEJIANG XIANJU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the related substances in the crude drug are detected according to the USP USP estrone content detection method, the following shortcomings are found: First, the USP method is isocratic elution, and the impurity F is less polar, and a high concentration is used in the mobile phase of the USP method Phosphate (50mM), cannot be eluted by gradient, impurity F cannot be eluted; second, impurity C is similar to estrone in structure, cannot be effectively separated, impurity C is not quantitatively accurate

Method used

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  • HPLC analysis method for estrone-related substances
  • HPLC analysis method for estrone-related substances
  • HPLC analysis method for estrone-related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Detection method:

[0047] Take an appropriate amount of estrone test sample, accurately weigh it, add acetonitrile-methanol (1:1) to dissolve and dilute it into a 4 mg / ml sample solution, shake well, accurately measure 5 μL and inject it into a liquid chromatograph, at a flow rate of 1.2 ml / ml. Min and column temperature of 40 ℃ for high performance liquid chromatography analysis, record the chromatogram.

[0048] The acetonitrile in mobile phase B was 60%.

[0049] Analyze the system suitability solution according to the following gradient stripping procedure,

[0050] time (min)

[0051] chromatogram see figure 1 , the retention time of each impurity and the main peak and the degree of separation between adjacent peaks are shown in Table 1.

[0052] Table 1

[0053] Sample name

[0054] It can be seen from the data in Table 1: acetonitrile in mobile phase B is 60%; flow rate: 1.2ml / min; column temperature: 40°C, each impurity and the main peak...

Embodiment 2

[0056] Others are the same as in Example 1, except that:

[0057] The acetonitrile in mobile phase B is 65%;

[0058] Analyze system suitability solutions according to the following gradient stripping procedure

[0059] time (min)

[0060] chromatogram see figure 2 , the acetonitrile in mobile phase B is 65%, and the separation between each impurity and the main peak and between impurities and impurities is good.

Embodiment 3

[0062] Others are the same as in Example 1, except that:

[0063] The acetonitrile in mobile phase B is 55%;

[0064] Analyze system suitability solutions according to the following gradient stripping procedure

[0065] time (min)

Mobile phase A%

Mobile phase B%

0

58

42

18

58

42

20

30

70

29

30

70

30

58

42

35

58

42

[0066] chromatogram see image 3 , the acetonitrile in mobile phase B is 55%, and the separation between each impurity and the main peak and between impurities and impurities is good.

[0067] Comparing the chromatograms in the above three examples, the chromatographic conditions of Example 1 are selected as the preferred conditions, that is, the acetonitrile in the mobile phase B is 60%.

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Abstract

The invention belongs to the field of steroid hormone drug analysis methods, and particularly relates to an HPLC analysis method for estrone-related substances, wherein the main parameters comprise that a chromatographic column having an octyl silane bonded silica gel as a filler is selected, mobile phase gradient elution is performed, the mobile phase comprises water, methanol and acetonitrile, high performance liquid chromatography analysis is performed at an appropriate flow rate and an appropriate column temperature, and the chromatogram is recorded. According to the present invention, with the HPLC analysis method, the impurities in the estrone bulk drug can be subjected to effective elution, separation and quantitation, and can be completely separated from the main peak, and the analysis is rapid; and the method can be separately used for the detection of the related substance in estrone impurity A sample or estrone impurity D sample.

Description

technical field [0001] The invention belongs to the field of steroid hormone drug analysis methods, in particular to an HPLC analysis method for estrone related substances. Background technique [0002] Estrone (3-hydroxy-1,3,5(10)-triene, 17-estrone) belongs to estrogen and is an important pharmaceutical intermediate, which can be used to synthesize ethinyl estradiol or estradiol. derivative. [0003] In the determination of estrone related substances, the common impurities are six compounds of A, B, C, D, E and F. Among them, impurity A and impurity E are unconverted materials, and other impurities come from the production of raw materials. produced by-products. There is no detailed report on the HPLC detection method of estrone API related substances. If the related substances in the API are detected according to the USP estrone content detection method, the following shortcomings are found: First, the USP method is isocratic elution, while the impurity F is less polar...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 李金涛王咏李杰
Owner ZHEJIANG XIANJU PHARMA
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