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Sterides compound analysis method

An analytical method and compound technology, applied in the direction of analytical materials, material separation, measurement devices, etc., to achieve high feasibility, good applicability, and good stability.

Inactive Publication Date: 2009-07-01
TIANJIN JINYAO GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Experimental program
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Effect test

Embodiment 1

[0042] Chromatographic conditions:

[0043] Chromatographic column: C18; 5μm; 4.6mm×250mm.

[0044] Mobile phase: acetonitrile: water = 43:57 (volume ratio)

[0045] Injection volume: 50μl

[0046] Detection wavelength: 240nm

[0047] Flow rate: 1.0ml / min

[0048] Operation: Take an appropriate amount of the sample, accurately weigh it, add acetonitrile to dissolve it and dilute it quantitatively to make a solution containing 0.4mg per 1ml, shake it up, accurately measure 50μl into the liquid chromatograph, record the chromatogram, and get the normalization of the sample Method liquid content.

[0049] Sample: The same batch number (060501) of halmethasone and the intermediates involved in its synthesis. The liquid phase results are shown in the attachment Figure 1-5 .

[0050]

Embodiment 2

[0052] Chromatographic conditions:

[0053] Chromatographic column: C18; 5μm; 4.6mm×250mm.

[0054] Mobile phase: acetonitrile-water (4:6)

[0055] Injection volume: 50μl

[0056] Detection wavelength: 240nm

[0057] Flow rate: 1.0ml / min

[0058] Operation: Take an appropriate amount of halmethasone sample 6, accurately weigh, add acetonitrile to dissolve and quantitatively dilute to make a solution containing 0.8mg per 1ml, shake well, accurately measure 50μl into the liquid chromatograph, record the chromatogram; Liquid content of normalization method.

[0059] Sample 6 and sample 1 are the same batch of halmethasone, the obtained liquid content: 98.96%, retention time (min): 17.732, the obtained HPLC chart is attached. Figure 6 .

Embodiment 3

[0061] Chromatographic conditions:

[0062] Chromatographic column: C18; 5μm; 4.6mm×250mm.

[0063] Mobile phase: acetonitrile-water (48:52)

[0064] Injection volume: 50μl

[0065] Detection wavelength: 245nm

[0066] Flow rate: 1.0ml / min

[0067] Operation: Take an appropriate amount of halmethasone sample 7, accurately weigh, add acetonitrile to dissolve and quantitatively dilute to make a solution containing 0.2mg per 1ml, shake up, accurately measure 50μl into the liquid chromatograph, record the chromatogram; Normalization method liquid content.

[0068] Sample 7 and sample 1 are the same batch of halmethasone, the obtained liquid content: 99.06%, retention time (min): 9.107, the obtained HPLC chart is attached Figure 7 .

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Abstract

An analysis method of steroid compound relates to an analysis method for Halometasone serial compounds and the intermediates in its synthesis, to provide a novel Halometasone liquid phase analysis method, which can systematically analyze Halometasone serial compounds and the intermediates in its synthesis.

Description

Technical field [0001] The present invention relates to analysis methods of halmethasone series compounds and some intermediates involved in their synthesis. Background technique [0002] Halometasone is a potent topical glucocorticoid drug containing halogen groups. It has rapid anti-inflammatory, anti-allergic, anti-itch, vasoconstriction, anti-exudation and anti-proliferative effects. It has strong activity and fast action, and is widely used in different types The inflammatory skin disease can quickly reduce and eliminate symptoms such as itching. [0003] There have been many reports on halmethasone, but the relevant reports on its analysis methods mainly involve only one analysis method of its preparations. A brief introduction is as follows: [0004] The literature Cesko-Slovenska Farmacie (1986), 35(6), 265-9. It is mentioned that the use of differential pulse polarography (differential pulse polarography; DPP) method for the treatment of hamethasone in ointment, cream an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/28
Inventor 朱润芝樊娜
Owner TIANJIN JINYAO GRP
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