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Method for extracting and separating flavonoid components in lindera aggregata leaves

A technology of black medicine leaves and ketones, which is applied in the field of separation and purification, can solve the problems of large solvent consumption, no extraction, separation and purification of chemical components, and reduced efficiency of the extraction, separation and purification process, and achieves good separation effect, less impurities, and purity. high effect

Active Publication Date: 2021-12-21
宁波市中医院
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the separation and purification efficiency of countercurrent chromatography is high, the extraction method is time-consuming and labor-intensive, the solvent consumption is large, and sometimes cumbersome enrichment treatment is required for the crude extract, which reduces the efficiency of the entire extraction, separation and purification process
[0005] Matrix solid-phase dispersion extraction (MSPD, matrix solid-phase dispersion) is a new type of sample pretreatment technology, which integrates extraction and purification into one step, and has the advantages of less solvent consumption , less environmental pollution, short extraction time, easy operation, high extraction efficiency, etc., has been widely used in the quantitative analysis of food, environmental samples, and traditional Chinese medicine, but there is no report on its use in the extraction, separation and purification of chemical components

Method used

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  • Method for extracting and separating flavonoid components in lindera aggregata leaves
  • Method for extracting and separating flavonoid components in lindera aggregata leaves
  • Method for extracting and separating flavonoid components in lindera aggregata leaves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] Embodiment 1: the selection of adsorbent kind

[0076] In parallel, 30 mg of 4 parts of black herb leaf powder were weighed and added to 4 groups of agate mortars, and 30 mg of different adsorbents (Florida Sillica (Ningbo Hongpu Instrument Technology Co., Ltd.), molecular sieve SBA-15 (Nanjing Jicang Nanotechnology Co., Ltd.) Ltd.), Al 2 o 3 (Shanghai Anpu Experimental Technology Co., Ltd.), Sillica gel (Shanghai Anpu Experimental Technology Co., Ltd.), respectively added to 4 groups of mortars and grinded for 3 minutes with the powder of black leaves. Pass the ground solid mixture through the matrix solid-phase column (with a gasket), add 2mL of 70% ethanol for pressure elution, collect the eluate, concentrate, and finally add 1mL of methanol to dissolve, at a speed of 13000rpm Centrifuge for 5 minutes with a centrifuge, collect and centrifuge to obtain the supernatant, take the supernatant and put it into a sample bottle, and perform detection and analysis with a h...

Embodiment 2

[0078] Embodiment 2: the selection of the mass ratio of sample and adsorbent

[0079] Weigh 30 mg of 4 parts of Aegina leaf powder in parallel, add them to 4 groups of agate mortars, and weigh silica gel with different masses (0 mg, 15 mg, 30 mg, 60 mg), add them into 4 groups of mortars and grind them 3min. Pass the ground solid mixture through the matrix solid-phase column (with a gasket), add 2mL of 70% ethanol for pressure elution, collect the eluate, concentrate, and finally add 1mL of methanol to dissolve, at a speed of 13000rpm Centrifuge for 5 minutes with a centrifuge, collect and centrifuge to obtain the supernatant, take the supernatant and put it into a sample bottle, and perform detection and analysis with a high-performance liquid chromatograph.

[0080] The extraction effects of different mass ratios of sample to adsorbent are as follows: Figure 2b As shown, the results show that the extraction efficiency of the target analyte increases gradually when the mas...

Embodiment 3

[0081] Embodiment 3: Elution solvent type selection

[0082] Weigh in parallel 6 parts of 30 mg of black herb leaf powder and 6 parts of 30 mg of silica gel, add them into two groups of agate mortars, and grind them for 3 minutes respectively. The ground solid mixture is passed through the matrix solid-phase small column (pad), add 2mL of ethanol, 70% ethanol, methanol, 50% methanol, 70% methanol, 90% methanol, preferably 70% ethanol eluent, add The eluate was collected and concentrated, and finally 1 mL of 70% methanol was added to dissolve it, centrifuged at 13,000 rpm for 5 min, collected and centrifuged to obtain the supernatant, and the supernatant was put into a sample bottle and used High-performance liquid chromatography for detection and analysis.

[0083] The extraction effects of different elution solvent types are as follows: Figure 2c Shown, result shows, 70% ethanol is higher than methanol, 50% methanol, 70% methanol, 90% methanol, ethanol, preferably 70% etha...

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Abstract

The invention discloses a method for extracting and separating flavonoid components in lindera aggregata leaves. The method comprises the following steps: mixing the lindera aggregata leaves with an adsorbent, performing eluting by adopting a matrix solid-phase dispersion extraction method, and performing concentrating to obtain a lindera aggregata leaf extract; performing primary separation and secondary separation treatment on the lindera aggregata leaf extract by adopting a high-speed counter-current chromatography, so as to realize separation of quercetin-3-O-beta-D-arabinofuranoside, a mixture of quercetin-3-O-beta-D-glucoside and quercetin-5-O-beta-D-glucoside, quercetin-3-O-rhamnopyranoside and kaempferol-7-O-alpha-L-rhamnopyranoside, wherein a second solvent system adopted in the secondary separation treatment comprises ethyl acetate, n-butyl alcohol, a resolving agent and water, and the resolving agent comprises cyclodextrin. According to the method provided by the invention, the flavonoid components purified and separated from the lindera aggregata leaves have the advantages of short separation period, high separation efficiency and few impurities.

Description

technical field [0001] The invention belongs to the technical field of separation and purification, and relates to a method for extracting and separating flavonoids from the leaves of argyria twigs, in particular to a method for extracting and separating flavonoids from leaves of agraceae based on solid-phase extraction combined with high-speed countercurrent chromatography with high efficiency and high recovery rate method of ingredients. Background technique [0002] Lindera aggregata (Sims) Kosterm is a plant of the genus Lindera in the family Lauraceae. It is distributed in Jiangsu, Zhejiang, Taiwan, Fujian, Guangdong and other provinces. It is most famous in Tiantai County, Zhejiang Province. It is called Tiantai Wuyao, Tiantai The output of black medicine accounts for 30% of the national black medicine products. Pharmacopoeia includes its dried roots as medicine. And its stems and leaves are used among the people. Among them, Wuyao Ye has been approved by the Health...

Claims

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Application Information

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IPC IPC(8): C07H1/08C07H17/07
CPCC07H1/08C07H17/07B01D15/1807Y02A50/30B01D2215/028
Inventor 彭昕楚楚邹艳芳童胜强
Owner 宁波市中医院
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