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Method for detecting content of hydrazine substance in steroid hormone substance

A technology for steroid hormones and substance content, which is applied in measuring devices, instruments, scientific instruments and other directions to achieve the effects of high sensitivity, good selectivity and good accuracy

Inactive Publication Date: 2021-03-09
HUNAN NORCHEM PHARMACEUTICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no analytical method for the content determination of hydrazines in abiraterone acetate, which is not publicly reported at home and abroad

Method used

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  • Method for detecting content of hydrazine substance in steroid hormone substance
  • Method for detecting content of hydrazine substance in steroid hormone substance
  • Method for detecting content of hydrazine substance in steroid hormone substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A method for detecting the content of hydrazines in steroid hormones, comprising the steps of,

[0035] 1. The chromatographic column is Agela promosil C18 250*4.6mm, 5μm particle size or similar chromatographic column.

[0036] 2. The detection wavelength is 305nm, which is the wavelength at which the hydrazine hydrate derivative (benzaldehyde azine) has greater absorption in the ultraviolet-visible region.

[0037] 3. The preferred mobile phase is 0.3g / L edetate sodium solution-acetonitrile (30:70).

[0038] 4. The analysis time is 20 minutes.

[0039] 5. The content of benzaldehyde azine was calculated by the external standard method; the injection volume was 40ul; the flow rate was 1.0ml / min; the column temperature was room temperature.

[0040] 6. Benzaldehyde azine reference substance solution: Accurately weigh 25 mg of hydrazine sulfate reference substance, put it in a 100mL measuring bottle, add diluent to dissolve and dilute to the mark, shake well, accuratel...

experiment example

[0046] 1. Sample recovery data

[0047]

[0048] 2. Selective

[0049] By adding an equal amount of the reference substance solution to the system suitability mixture, and comparing the peak area of ​​the hydrazine sulfate derivative with the reference substance solution, it is concluded that there is no influence on the detection of hydrazine hydrate under the condition that other impurities exist.

[0050] The peak area of ​​hydrazine sulfate derivative in the reference substance solution ( Figure 4 ): 11508.55;

[0051] The peak area of ​​hydrazine sulfate derivative in the system suitability solution ( Figure 5 ): 11255.81.

[0052] 3. Sensitivity

[0053] The limit of quantification of the method was calculated to be about 0.03ppm by the signal-to-noise ratio of the limit of quantification not less than 10:1. Has a high sensitivity.

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Abstract

The invention relates to a method for detecting the content of hydrazine substances in a steroid hormone substance, which comprises the following steps of: preparing a test solution, namely, weighinga steroid hormone substance containing hydrazine substances, adding a diluent, dispersing, adding benzaldehyde, uniformly mixing, adding an extracting agent, stirring, standing for layering, and taking a supernatant to obtain the test solution, the diluent being a mixed solution of diluted hydrochloric acid and ethanol, and the weight concentration of the diluted hydrochloric acid being 9.5-10.5%;preparing a hydrazine substance reference substance solution; determining chromatographic conditions: using octadecylsilane as a stationary phase, selecting a mobile phase for isocratic elution, andcontrolling the detection wavelength at 300-340 nm, and enabling the mobile phase to be 0.3g / L sodium edetate solution-acetonitrile; and determining the content of hydrazine substances. The method isgood in selectivity, high in accuracy and high in sensitivity.

Description

technical field [0001] The invention belongs to the field of detection of organic substance content, and in particular relates to a method for detecting the content of hydrazine substances in steroid hormone substances. Background technique [0002] In the production process of abiraterone acetate, hydrazine hydrate was used in the reaction process of the synthesis of intermediate I (3β-alcohol-5,16-diene-17-hydrazone androst), and the hydrazines belong to the warning structure Genotoxic impurities, extremely low limit requirements for genotoxic impurities, pose a higher challenge to the process and detection analysis, and also become a technical challenge and potential barrier for drugs to enter the European and American markets. In order to strictly control product quality, the finished product of abiraterone acetate Monitor the content of hydrazine substances in the system to prevent unqualified products from entering the market. At present, there is no publicly reported...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/36G01N30/74G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/36G01N30/74G01N30/8679G01N2030/045G01N2030/067
Inventor 张跃王诗盛李林梅靳志忠曾春玲
Owner HUNAN NORCHEM PHARMACEUTICAL CO LTD
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