Method for separating and purifying quercetin tagetin from marigold

A technology for separation and purification of quercetin marigold, which is applied in the direction of organic chemistry, can solve the problems of unsuitable separation and purification of substances with complex components, unsuitable for industrialized large-scale production, and lack of repeatability, so as to shorten the preparation time and batch High degree of consistency between times and the effect of reducing column elution time

Active Publication Date: 2018-07-24
TIANJIN YAOYU BIOLOGICAL TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The paper "Isolation and Structural Identification of Tagetin and Quercetin Tagetin" (Journal of Guangzhou Medical College, Volume 18, No. 1, 1990) proposed that quercetin tagetin crystals could be obtained by organic solvent extraction and recrystallization. However, the crystallization is obtained through multiple extractions and multiple recrystallizations. Not only is the operation complicated, the workload is heavy, and the cost is high. More importantly, this method is not repeatable and is not suitable for industrialized large-scale production.
[0005] The Chinese invention patent with the publication number CN102190646B also discloses a preparation method of quercetin tagetin, which proposes to use a preparative high-speed countercurrent chromatography for extraction, and the purity of the quercetin tagetin obtained can reach more than 95%, but the The method has limited separation components and low separation efficiency, and is not suitable for the separation and purification of substances with complex components such as whole marigold flowers

Method used

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  • Method for separating and purifying quercetin tagetin from marigold
  • Method for separating and purifying quercetin tagetin from marigold
  • Method for separating and purifying quercetin tagetin from marigold

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Embodiment 1

[0036] The method for separating and purifying quercetin tagetin from marigold in this embodiment comprises the following steps:

[0037] Take dried marigold flowers as raw materials, grind them into powder, extract and rotary steam with ethanol to obtain dried marigold coarse powder, weigh 5g, dissolve in 50mL of 95% methanol-water solution, and prepare a marigold extract solution with a concentration of 100mg / mL, passed through a 0.45 μm microporous membrane, and prepared by one-dimensional liquid chromatography. One-dimensional liquid chromatography using reversed-phase column DAISO C 18 (250mm×20mmi.d., 8μm), the mobile phase is a mixture of organic phase and water phase, wherein phase A is water, phase B is methanol, isocratic elution method: concentration of phase B is 53% isocratic for 20min. Using UV detector 210nm and 260nm as dual selective absorption wavelengths, preparation temperature is room temperature, injection volume is 500μL / needle, mobile phase flow rate ...

Embodiment 2

[0040] The method for separating and purifying quercetin tagetin from marigold in this embodiment comprises the following steps:

[0041] Take dried marigold flowers as raw materials, grind them into powder, extract and rotary steam with ethanol to obtain dried marigold coarse powder, weigh 5g, dissolve it in 100mL 95% methanol-water solution, and prepare a marigold extract solution with a concentration of 25mg / mL, passed through a 0.45 μm microporous membrane, and prepared by one-dimensional liquid chromatography. One-dimensional liquid chromatography using reversed-phase column DAISO C 18 (250mm×20mmi.d., 8μm), the mobile phase is a mixture of organic phase and water phase, wherein A phase is water, B phase is methanol, isocratic elution method: B phase concentration 55% isocratic 20min, 0 % isocratic for 10 min. Adopting ultraviolet detector 210nm and 260nm as dual selective absorption wavelengths, preparation temperature is room temperature, injection volume is 500 μ L / ...

Embodiment 3

[0044] Take dried marigold flowers as raw materials, grind them into powder, extract and rotary steam with ethanol to obtain dried marigold coarse powder, weigh 5g, dissolve in 25mL 95% methanol-water solution, and prepare marigold extract solution with a concentration of 200mg / mL, passed through a 0.45 μm microporous membrane, and prepared by one-dimensional liquid chromatography. One-dimensional liquid chromatography using reversed-phase column DAISO C 18 (250mm×20mmi.d., 8μm), the mobile phase is a mixture of organic phase and water phase, wherein A phase is water, B phase is methanol, isocratic elution method: B phase concentration 50% isocratic 20min, 100 % isocratic for 10 min. Adopting ultraviolet detector 210nm and 260nm as dual selective absorption wavelengths, preparation temperature is room temperature, injection volume is 500 μ L / needle, mobile phase flow rate is 12mL / min, according to ultraviolet absorption spectrum ( Figure 7 As shown), the fractions collecte...

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Abstract

The invention provides a method for separating and purifying quercetin tagetin from marigolds, which comprises the following steps: drying the dried flowers of marigolds and grinding them into powder, soaking them in ethanol or extracting them under reflux, rotating the filtered filtrate to dryness, and dissolving In a mixed solvent of methanol-water; perform one-dimensional liquid chromatography: use DAISO C18 as a chromatographic column, phase A water and phase B methanol as mobile phase, phase B concentration 50-55% isocratic elution for 20min, according to the ultraviolet absorption spectrum Collect the eluate after 6-12 minutes as the target component, and then dissolve it in methanol-water mixed solvent after rotary evaporation to dryness; carry out two-dimensional liquid chromatography: use Acchrom X-Amide as the chromatographic column, A phase water, B phase acetonitrile It is the mobile phase, and the B phase concentration is 92-98% and isocratic elution for 40 minutes. According to the ultraviolet absorption spectrum, the 27-33-minute eluate is collected as the target component, and the quercetin-tagoldin with a purity of more than 99% is obtained by rotary evaporation to dryness. .

Description

technical field [0001] The invention relates to the technical field of extraction of effective plant components, in particular to a method for separating and purifying quercetin tagetes from marigolds. Background technique [0002] Marigold, also known as Chrysanthemum chrysanthemum, scientific name Tagetes erecta, belongs to the genus Marigold of Compositae, is an annual herbaceous plant, in addition to having ornamental value, it also has good medicinal value. Quercetagetin contained in marigold flowers is a flavonoid compound unique to marigolds, which has anti-inflammatory, anti-allergic, blood pressure-lowering, anti-arrhythmic, anti-platelet aggregation, and anti-oxidation effects. Its molecular formula is C 15 h 10 o 8 , the molecular weight is 318.237, and the structural formula is as follows: [0003] [0004] The paper "Isolation and Structural Identification of Tagetin and Quercetin Tagetin" (Journal of Guangzhou Medical College, Volume 18, No. 1, 1990) pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/30C07D311/40
Inventor 张耀洲陆洪
Owner TIANJIN YAOYU BIOLOGICAL TECH
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