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Method for separating and purifying naringin and neohesperidin from white skin layer of citrus grandis

A new hesperidin, separation and purification technology, applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve problems such as unfavorable mass production, low process efficiency, long production cycle, etc., and achieve safe and easy production process. The effect of simple operation and synthesis process and short production cycle

Active Publication Date: 2014-07-23
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, the extraction and separation of naringin and neohesperidin mainly use organic solvent extraction combined with crystallization, but these processes have low efficiency, long production cycle, serious pollution, and are not conducive to mass production
Recently, the macroporous resin method has become a new method of extracting and purifying flavonoids from citrus plants, which can separate and obtain high-purity flavonoids, but due to the neohesperidin, naringin and orange The physical and chemical properties of dermatosin and other compounds are very close. For plant materials containing these compounds at the same time, it is very difficult to separate them by a single method of macroporous resin.

Method used

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  • Method for separating and purifying naringin and neohesperidin from white skin layer of citrus grandis
  • Method for separating and purifying naringin and neohesperidin from white skin layer of citrus grandis
  • Method for separating and purifying naringin and neohesperidin from white skin layer of citrus grandis

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Embodiment 1

[0021] Example 1 The operation method of the present invention for separating and purifying naringin and neohesperidin is carried out according to the following two steps:

[0022] see figure 1 , (1) Preparation of macroporous resin crude extract powder: 8 g dried Huyou white cortex was extracted twice with 80% ethanol (solid-liquid ratio 1:25) ultrasonically (40 °C), centrifuged at 4000 rpm for 20 min, The two supernatants were combined and evaporated to dryness on a rotary evaporator to obtain the extract, which was dissolved in ddH 2 In O, about 200 mL of D101 macroporous resin was applied, the bed volume (BV) was 20 mL, and the sample flow rate was 2 mL / min. After loading, the D101 macroporous resin was first washed with water for 4 BV to remove impurities, then naringin and neohesperidin were eluted with 60% ethanol, and 8 BV were eluted until no naringin and neohesperidin could be detected in the effluent. Hesperidin, the elution flow rate was 2 mL / min, 60% of the elue...

Embodiment 2

[0025] The operation method of separating and purifying naringin and neohesperidin of the present invention is carried out according to the following two steps:

[0026] see figure 1 , (1) Preparation of macroporous resin crude extract powder: 16 g dried Huyou white cortex was extracted twice with 80% ethanol (solid-liquid ratio 1:25) ultrasonically (40 °C), centrifuged at 4000 rpm for 20 min, The two supernatants were combined and evaporated to dryness on a rotary evaporator to obtain the extract, which was dissolved in ddH 2 In O, about 400 mL of D101 macroporous resin was applied, the bed volume (BV) was 20 mL, and the sample flow rate was 2 mL / min. The loaded D101 macroporous resin was first washed with water for 4 BV to remove impurities, and then 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80% ethanol was used to elute naringin and 80% ethanol. Neohesperidin, washed 4 BV per gradient, the elution flow rate was 2 mL / min, combined 10%-60% eluent, evaporated to dryness on a rotary...

Embodiment 3

[0028] Example 3 The present invention screened and determined the influencing factors through the following tests

[0029] 1. Selection of purification materials

[0030] The fresh Huyou fruit is divided into four different parts: oil cell layer, white skin layer, capsule coat, and juice cell. The four different parts are dried in an oven at 50°C to constant weight, crushed with a sample mill, and passed through a 40-mesh sieve. Accurately weigh a certain amount of dry sample powder from four different parts of Huyou, extract with 80% ethanol (solid-to-liquid ratio 1:25) ultrasonically for 40 min (30°C), and centrifuge the extract on a centrifuge at 4000 rpm for 20 min, and repeat the process. Twice, the supernatants were pooled for HPLC analysis of naringin and neohesperidin. HPLC mobile phases include ddH 2 Chromatography of O (A) and acetonitrile (B) using isocratic elution of A:B=79:21, flow rate of 1 mL / min, and detection wavelength of 280 nm. The results showed that ...

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Abstract

The invention provides a method for separating and purifying naringin and neohesperidin from a white skin layer of citrus grandis, which comprises using combining technologies of macroporous resin and high-speed counter-current chromatography, and utilizing drying powder of the white skin layer of the citrus grandis to serve as a raw material, and first preparing macroporous resin crude extract powder; and obtaining the high-purity naringin and neohesperidin by further separation and purification through the high-speed counter-current chromatography. The method is simple to operate, does not need high temperature, high pressure and protection of inert gas and is simple in synthesizing process. A reagent which has strong sharp aroma does not need to be used, and the production process is safe and easy to operate. The method can be used for separating flavonoid compounds which are extremely approximate in using properties and is wide in applicability, short in production cycle and high in purification recovery rate, purity and accuracy. The using amount of samples is little, equipment investment is small, the conditions are stable and easy to control, and the finally purified naringin and the neohesperidin have the purity of over 95% and are suitable for industrial production and scientific research.

Description

technical field [0001] The invention belongs to the technical field of extraction, separation and purification of effective components in natural plants, and in particular relates to a method for simultaneously separating and purifying naringin and neohesperidin by using the white cortex of Huyou as a raw material and adopting the combined technology of macroporous resin and HSCCC. Background technique [0002] Naringin (naringin), alias naringin; citrus glycoside, isohesperidin, molecular formula: C 27 H 32 O 14 , molecular weight: 580.54, CAS number: 10236-47-2, belongs to the flavanones in flavonoids, and its glycoside ligand is 4 ， ,5,7-Trihydroxyflavone, the glycosyl is rhamnosyl β -1,2-Glucose. A glycoside present in the flowers and fruits of pomelo, lime, and is a bitter substance. Neohesperidin, molecular formula: C 28 H 34 O 15 , molecular weight: 610.56, CAS number: 13241-33-3, belongs to the flavanones in flavonoids, and its glycoside ligand is 3',5,7-trih...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/07C07H1/08
Inventor 孙崇德李鲜张九凯陈昆松
Owner ZHEJIANG UNIV
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