Method of separating and purifying polymethoxyflavone compounds from tangerine fruits

A technology for separating and purifying polymethoxyflavonoids is applied in the field of separating and purifying polymethoxyflavonoids from citrus fruits, and can solve the problems of high cost, low monomer purity, low preparation amount, complicated process, etc. Low, safe and easy to operate production process, simple process effect

Active Publication Date: 2017-08-04
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing separation of polymethoxylated flavonoids mainly adopts macroporous resin chromatography and preparative high-performance liquid chromatography. The limitations are that the process is complex, the cost is high, and the purity of the isolated monomers is low or the amount of preparation is difficult to develop into Separation technology with high separation purity and large preparation volume

Method used

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  • Method of separating and purifying polymethoxyflavone compounds from tangerine fruits
  • Method of separating and purifying polymethoxyflavone compounds from tangerine fruits
  • Method of separating and purifying polymethoxyflavone compounds from tangerine fruits

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Effect test

Embodiment 1

[0022] The operating method of the present invention for separating and purifying nobiletin, tangeretin and 5-nornobiletin is carried out according to the following steps, see figure 1 :

[0023] (1) Ultrasonic-assisted extraction: 10.3 g of freeze-dried Ou mandarin fruit peel powder was ultrasonically extracted three times (25°C) with 95% ethanol (solid-to-liquid ratio 1:20), each time for 45 minutes, after vacuum filtration, the supernatant was combined , evaporated to dryness on a rotary evaporator to an ethanol-free phase, and dissolved in deionized water to obtain an aqueous solution of the crude extract.

[0024] (2) C18 solid-phase extraction column for sugar removal and segmentation: take about 5 mL of the crude extract aqueous solution obtained in step (1) and load it C18 solid-phase extraction column, after loading, the solid-phase extraction column is first eluted with deionized water for 25 times of column bed volume (BV) to remove impurities with higher polar...

Embodiment 2

[0027] The operating method of the present invention for separating and purifying nobiletin, tangeretin and 5-nornobiletin is carried out according to the following steps, see figure 1 :

[0028] (1) Ultrasonic-assisted extraction: 11.2 g of freeze-dried Ou mandarin fruit peel powder was ultrasonically extracted three times with 95% ethanol (solid-to-liquid ratio 1:20) (25°C), each time for 45 minutes, vacuum filtered, and the supernatant was combined , evaporated to dryness on a rotary evaporator to an ethanol-free phase, and dissolved in deionized water to obtain an aqueous solution of the crude extract.

[0029] (2) C18 solid-phase extraction column for sugar removal and segmentation: take about 5 mL of the crude extract aqueous solution obtained in step (1) and load it C18 solid-phase extraction column, after loading, the solid-phase extraction column is first eluted with deionized water for 25 times of column bed volume (BV) to remove impurities with higher polarity, a...

Embodiment 3

[0031] Embodiment 3 The present invention carries out the screening determination of influence factor by following test

[0032] 1. Selection of purification materials

[0033] The peel of fresh Ou mandarin fruit is freeze-dried to constant weight and ground into powder with a mill. Take a certain quality of freeze-dried Ou mandarin peel powder and use 95% ethanol (solid-to-liquid ratio: 1:20) to ultrasonically extract for 45 minutes (25°C), repeat twice, and after vacuum filtration, combine the supernatant for multiple use. UPLC analysis of methoxylated flavonoids. The UPLC mobile phase includes deionized water (solution A) and chromatographic acetonitrile (solution B), using gradient elution, the detection wavelength is 330nm, the temperature is room temperature (25 ° C), the injection volume is 2 μl, and the flow rate is 0.3ml / min. The conditions are: solvent B: 0-5min, 20%, 5-8min: 20%-34%; 8-20min: 34%-60%, 20-22min: 60%-100%, 22~23min: 100% Change, 23-24min: 100%-20%,...

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Abstract

The invention provides a method of separating and purifying polymethoxyflavone compounds from tangerine fruits. By taking pericarp of the tangerine fruits as a raw material, the method finally obtains three high purity polymethoxyflavone compounds: nobiletin, tangeretin and 5-nor-nobiletin by adopting ultrasonic-assisted extraction and desaccharification and segmentation by a solid-phase extraction column (formula as shown in the description) by means of a high-speed countercurrent chromatography (HSCCC) purification and separation technology. The method without high temperature and high pressure and inert gas protection is simple to operate, short in production period, small in dosage of samples, stable and easy for condition control, short in production period and wide in adaptability; the purified product is high in recovery rate and high in purity, and the purities of the three compounds are 98% above; the used solvent can be recycled and repeatedly used, the cost is relatively low, and the purification process is precisely determined and quantified and high in accuracy; and the substance resolution ratio and reappearance degree of HSCCC can be improved. The method is suitable for industrial production and scientific research.

Description

technical field [0001] The invention belongs to the technical field of extracting, separating and purifying active ingredients in natural plants, and specifically relates to a method for separating and purifying polymethoxyflavonoids from Ou mandarin fruit. The combined technology of C18 solid phase extraction column and HSCCC (High Speed ​​Counter-Current Chromatography) simultaneously separates and purifies three polymethoxyflavonoids of nobietin, tangeretin and 5-nornobiletin. Background technique [0002] Ou mandarin (Citrus reticulata cv. Suavissima) is a cultivated variety of Rutaceae Citrus, and it is also a traditional specialty product in Wenzhou and Lishui, Zhejiang Province. It has been cultivated for more than two thousand years. Ou tangerine has special food and medicine functions such as anti-tumor, heat-removing and fluid-reducing, phlegm-relieving and cough-relieving, cooling and detoxifying among the people. These effects may be related to the rich polymeth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30C07D311/40
Inventor 孙崇德王岳陈昆松李鲜曹锦萍
Owner ZHEJIANG UNIV
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