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Impurity A in troxerutin and separation method thereof

A separation method and impurity technology, applied to the field of impurity A in troxerutin and its separation, capable of solving problems such as adverse reactions

Active Publication Date: 2015-05-20
SUZHOU YABAO PHARMA R&D CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Impurities and harmful substances produced during the preparation process can cause adverse reactions

Method used

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  • Impurity A in troxerutin and separation method thereof
  • Impurity A in troxerutin and separation method thereof
  • Impurity A in troxerutin and separation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Example 1 : Separation of Impurity A from Troxerutin

[0048] Equipment: Agela Technologies CHEETAH HP-100

[0049] Chromatographic column: spherical silica gel, 15μm, 200mm×60mmID

[0050] Mobile phase: A isopropanol: B water = 50:1

[0051] Duty ratio: 100

[0052] Column pressure: 0.1MPa

[0053] Flow rate: 50ml

[0054] Detection wavelength: 254nm

[0055] Injection volume: 1g / injection

[0056] After dissolving troxerutin with the mobile phase, load it on the chromatographic column, and then use the mobile phase to elute and separate. After washing, the organic phase was concentrated to dryness under reduced pressure to obtain a yellow solid with a purity of 99%. Acid hydrolysis TLC detection, containing glucose and rhamnose. MS(ESI) calcd for [M+H] detected by mass spectrometry + :713.1, which is impurity A.

[0057] Separation of Narcisin from Rutin

[0058] Equipment: Agela Technologies CHEETAH HP-100

[0059] Chromatographic column: spherical ...

Embodiment 2

[0067] Embodiment 2: Narciscin in rutin produces impurity A

[0068] Equipment: Agela Technologies CHEETAH HP-100

[0069] Chromatographic column: spherical silica gel, 15μm, 200mm×60mmID

[0070] Mobile phase: A dichloromethane: B methanol = 200:1

[0071] Duty ratio: 150

[0072] Column pressure: 0.1MPa

[0073] Flow rate: 100ml

[0074] Detection wavelength: 254nm

[0075] Injection volume: 10g / injection

[0076] After dissolving the crude rutin with the mobile phase, load it on the chromatographic column, then elute and separate it with the mobile phase, collect the eluate in sections, and concentrate it to dryness under reduced pressure to obtain pure rutin with a purity of ≥98% and does not contain Narcisin.

[0077] Put 10.0 g of enriched pure rutin (purity ≥ 98%, does not contain narcissin) into a reaction vessel, add 40 ml of methanol, 0.1 g of sodium hydroxide, and 4 g of ethylene oxide, stir and heat to 100 ° C for reaction, 3 hours, troxerutin was obtaine...

Embodiment 3

[0087] Example 3 Mobile Phase Screening of Troxerutin Impurity A Separation Method

[0088] Equipment: Agela Technologies CHEETAH HP-100

[0089] Chromatographic column: spherical silica gel, 15μm, 200mm×60mmID

[0090] Duty ratio: 150

[0091] Column pressure: 0.1MPa

[0092] Flow rate: 50ml

[0093] Detection wavelength: 254nm

[0094] Injection volume: 1g / injection

[0095] Table 2 Screening of different mobile phases

[0096]

[0097] Troxerutin was dissolved in the mobile phase, loaded on the chromatographic column, and then eluted and separated with different mobile phases in Table 1. The eluate was collected in sections, concentrated under reduced pressure to dryness, and the concentrated solution was dissolved in dichloromethane. Washed with saturated citric acid, the organic phase was concentrated to dryness under reduced pressure to obtain a yellow solid.

[0098] It can be seen from the above experiments that the mobile phase is isopropanol: water, and w...

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Abstract

The invention discloses a novel impurity A and a method for separating the impurity A from troxerutin, further researches that the impurity A is introduced by narcissoside in rutin, and discloses a separation method of narcissoside so as to provide reference for further reducing the content of the impurity A in the troxerutin. By adopting the separation method disclosed by the invention, the purity of the impurity A is at least 95%, and the purity of the narcissoside is at least 95%.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular to an impurity A in troxerutin and a separation method thereof. Background technique [0002] Troxerutin is a mixture of semi-synthetic flavonoids made from rutin through hydroxyethylation, suitable for hemiplegia, aphasia and pre-myocardial infarction syndrome, arteriosclerosis, central Retinitis, thrombophlebitis, varicose veins, edema caused by increased vascular permeability, etc. Currently listed preparations include tablets, injections, capsules, and oral liquids. [0003] On September 20, 2014, the national drug standard for troxerutin was updated. Under the other component testing items in the standard, it is required that in troxerutin for injection, monohydroxyethylrutin peak, dihydroxyethyl The peak areas of rutin and tetrahydroxyethyl rutin shall not be greater than 5.0% of the total peak area, the peak areas of other single unknown components shall not be greater th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/06
CPCC07H1/06C07H17/07
Inventor 彭涛吕立天
Owner SUZHOU YABAO PHARMA R&D CO LTD
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