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Impurity detection analysis method of norethisterone derivatives and intermediates thereof

An analysis method and intermediate technology, applied in the field of impurity analysis of steroid compounds, to achieve the effect of improving detection efficiency and short detection time

Active Publication Date: 2016-01-27
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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  • Impurity detection analysis method of norethisterone derivatives and intermediates thereof
  • Impurity detection analysis method of norethisterone derivatives and intermediates thereof
  • Impurity detection analysis method of norethisterone derivatives and intermediates thereof

Examples

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Effect test

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: 10μL

[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 i...

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: 10μL

[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 invention relates to an impurity analysis method of a steroid compound, and especially relates to an impurity detection analysis method of norethisterone derivatives and intermediates thereof. The method comprises the following steps: (1) a chromatographic column with octadecylsilane chemically bonded silica as a filler is selected; a mobile phase gradient elution is carried out, and the mobile phase contains water, methanol and acetonitrile; the detection wavelength is 230-254nm; and (2) a proper amount of the test sample norethisterone derivatives or intermediates thereof are selected, methanol is precisely weighed for dissolving and diluting the test sample to form a sample solution of a certain concentration, the solution is uniformly shaken, and a high performance liquid chromatography analysis is carried out at a proper flow velocity and a proper column temperature, in order to record a chromatogram. The method can be used for rapidly and accurately realizing impurity analysis of norethisterone derivatives, and is especially suitable for the impurity analysis of norethisterone enanthate, and simultaneously can be used for impurity analysis of norethisterone derivative intermediates, and can be used for effectively tracing impurities generated in the synthesis process.

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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IPC IPC(8): G01N30/02
Inventor 王咏芦飞李文君
Owner ZHEJIANG XIANJU PHARMA
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