A kind of impurity detection and analysis method of norethindrone derivative and its intermediate

An analytical method and intermediate technology are applied in the field of impurity analysis of steroid compounds to achieve the effects of improving detection efficiency and shortening detection time.

Active Publication Date: 2017-06-23
ZHEJIANG XIANJU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the research objects in the existing public literature are the preparation content detection methods of norethindrone enanthate, or the use of liquid mass spectrometry detection methods to detect alkynyl steroid compounds. For potential impurities in the actual production process of raw materials, such as intermediates , degradation products, etc. are not involved, and there is no related impurity analysis method that can be applied to the impurity detection of norethindrone derivative products and intermediates involved in the synthesis of such products

Method used

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  • A kind of impurity detection and analysis method of norethindrone derivative and its intermediate
  • A kind of impurity detection and analysis method of norethindrone derivative and its intermediate
  • A kind of impurity detection and analysis method of norethindrone derivative and its intermediate

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Embodiment 1

[0083] A method for detecting and analyzing impurities of norethindrone derivatives and intermediates thereof:

[0084] (1) Chromatographic conditions:

[0085] Chromatographic column: C18, 4.6mm×25cm, 5µm

[0086] Detection wavelength: 240nm

[0087] Injection volume: 10 μL

[0088] Flow rate: 1.5ml / min

[0089] Column temperature: 30°C

[0090] Mobile phase: water, methanol and acetonitrile,

[0091] (2) Analyze according to the following operation method, and the program gradient elution is the same as in Table 1.

[0092] Operation: Accurately weigh an appropriate amount of samples 1-6 of norethindrone derivatives or intermediates involved in their synthesis, place them in a volumetric flask, add methanol to dissolve and dilute to the mark, and make a solution containing 1mg of samples per 1ml, shake well , Precisely measure 10 μL and inject it into the liquid chromatograph, and record the chromatogram. See attached chromatogram Figure 1~6 , the results are shown ...

Embodiment 2

[0099] A kind of impurity detection analysis method of norethindrone enanthate:

[0100] (1) Chromatographic conditions:

[0101] Chromatographic column: C18, 4.6mm×25cm, 5µm

[0102] Detection wavelength: 230nm

[0103] Injection volume: 10 μL

[0104] Flow rate: 1.3ml / min

[0105] Column temperature: 40°C

[0106] Mobile phase: water, methanol and acetonitrile

[0107] (2) Analyze according to the following operation method, and the program gradient elution is the same as in Table 1.

[0108] Operation: Accurately weigh an appropriate amount of norethindrone enanthate sample 7, put it in a volumetric flask, add methanol to dissolve and dilute to the mark, make a solution containing 1mg of sample per 1ml, shake well, accurately measure 10μL and inject it into the liquid chromatograph , record the chromatogram. See attached chromatogram Figure 7 , the results are shown in Table 4.

[0109] Table 4

[0110]

[0111] From the results in Table 4, it can be seen that...

Embodiment 3

[0113] A kind of impurity detection analysis method of norethindrone enanthate:

[0114] (1) Chromatographic conditions:

[0115] Chromatographic column: C18, 4.6mm×25cm, 5µm

[0116]Detection wavelength: 254nm

[0117] Injection volume: 10μL

[0118] Flow rate: 1.0ml / min

[0119] Column temperature: 25°C

[0120] Mobile phase: water, methanol and acetonitrile,

[0121] (2) Program gradient elution according to Table 5

[0122] table 5

[0123]

[0124] Operation: Accurately weigh an appropriate amount of norethindrone enanthate sample 8, put it in an appropriate volumetric flask, add methanol to dissolve and dilute to the mark, make a solution containing 1 mg of sample per 1 ml, shake well, accurately measure 10 μL and inject into the liquid chromatograph, Record the chromatogram. See attached chromatogram Figure 8 , the results are shown in Table 6.

[0125] Table 6

[0126]

[0127] From the results in Table 6, it can be seen that when the method is used f...

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Abstract

The present invention relates to a method for analyzing impurities of steroidal compounds, in particular to a method for detecting and analyzing impurities of norethindrone derivatives and their intermediates, comprising: (1) choosing octadecylsilane bonded silica gel as filler The chromatographic column; the gradient elution of the mobile phase, the composition of the mobile phase is water, methanol and acetonitrile; the detection wavelength is 230 ~ 254nm; (2) take the test sample norethindrone derivative or its intermediate amount, accurately weigh the methanol Dissolve and dilute to a certain concentration of the sample solution, shake it up, inject the sample, perform high-performance liquid chromatography analysis at an appropriate flow rate and column temperature, and record the chromatogram. The invention can quickly and accurately realize the impurity analysis of norethindrone derivatives, especially for the impurity analysis of norethindrone enanthate, and can be used for the impurity analysis of norethindrone derivative intermediates, and can effectively track the impurities produced in the synthesis process. Impurities.

Description

technical field [0001] The invention relates to a method for analyzing impurities of steroidal compounds, in particular to a method for detecting and analyzing impurities of norethindrone derivatives and intermediates thereof. Background technique [0002] Norethindrone drugs are a class of progestogens that can be used to treat premenstrual syndrome, dysmenorrhea, excessive menstrual bleeding, abnormal menstruation, and menopausal syndrome. They are also commonly used as oral short-acting contraceptives. Norethindrone is the first oral high-efficiency progestogen that can be synthesized, and its esterified derivatives have the same pharmacological effects, but also prolong the time of action. Common norethindrone esterified derivatives include norethindrone acetate, norethindrone caproate, norethindrone enanthate, norethindrone octanoate, etc., wherein norethindrone enanthate and estradiol valerate compound injection Effective contraceptives can continue to prevent pregnan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 王咏芦飞李文君
Owner ZHEJIANG XIANJU PHARMA
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