A kind of hplc analysis method of related substances of estrone

An analysis method and technology for related substances, which are applied in the field of HPLC analysis of estrone related substances, can solve the problems of inaccurate quantification of impurity C, inability to elute and effectively separate impurity F, etc., and achieve accurate determination and fast analysis speed. Effect

Active Publication Date: 2020-08-25
ZHEJIANG XIANJU PHARMA
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  • Description
  • Claims
  • Application Information

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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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  • A kind of hplc analysis method of related substances of estrone
  • A kind of hplc analysis method of related substances of estrone
  • A kind of hplc analysis method of related substances of estrone

Examples

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Comparison scheme
Effect test

Embodiment 1

[0046] Detection method:

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

[0048] Acetonitrile in mobile phase B was 60%.

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

[0050] 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

[0051] 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.

[0052] Table 1

[0053] Sample name code name retention time (min) Resolution between adjacent peaks ADD Impurity...

Embodiment 2

[0056] Others are the same as embodiment 1, the difference is:

[0057] Acetonitrile in mobile phase B is 65%;

[0058] Analyze the system suitability solution according to the following gradient elution procedure

[0059] 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

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

Embodiment 3

[0062] Others are the same as embodiment 1, the difference is:

[0063] Acetonitrile in mobile phase B is 55%;

[0064] Analyze the system suitability solution according to the following gradient elution 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 , acetonitrile in the mobile phase B was 55%, and all impurities were well separated from the main peak and between impurities.

[0067] The chromatograms in the above 3 examples are compared, and the chromatographic conditions of the selected example 1 are preferred conditions, that is, 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 related substances of estrone, 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. For the HPLC detection method of related substances of estrone bulk drug, there is no detailed report. 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 im...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 李金涛王咏李杰
Owner ZHEJIANG XIANJU PHARMA
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