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Method for separating and purifying seven flavonoid compounds from tangerine oil vacuole layer

A flavonoid compound, separation and purification technology is applied in the field of extraction, separation and purification of effective components in natural plants, can solve the problems of low process efficiency, long production cycle, unfavorable production and the like, and achieves simple synthesis process, short production cycle and recovery rate. high effect

Inactive Publication Date: 2014-03-05
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 citrus flavonoids 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

Method used

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  • Method for separating and purifying seven flavonoid compounds from tangerine oil vacuole layer
  • Method for separating and purifying seven flavonoid compounds from tangerine oil vacuole layer
  • Method for separating and purifying seven flavonoid compounds from tangerine oil vacuole layer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1 The present invention carries out the screening determination of influence factor by following test

[0016] 1. Selection of purification materials

[0017] Fresh Ou mandarin fruit is divided into four parts: oil cell layer, white cortex, capsule, and juice sac. After being fully freeze-dried in liquid nitrogen, dry it in a freeze dryer at -80°C for 72 h to constant weight. The dry sample is crushed Grinding machine for use. Accurately weigh a certain amount of dry sample powder from four different parts of Ou mandarin, ultrasonically extract with 80% ethanol (solid-to-liquid ratio 1:20) for 30 min, and centrifuge the extract at 4000 rpm for 10 min in a centrifuge, repeat this twice, and combine The supernatant was used for HPLC analysis of flavonoids in four different parts of Ougan fruit. The HPLC analysis conditions are: water (solution A) and chromatographic acetonitrile (solution B) are used as mobile phases, gradient elution is adopted, the elutio...

Embodiment 2

[0028] The method for the separation and purification of flavonoids in the oil cell layer of Ou mandarin orange according to the present invention is carried out according to the following three steps, see figure 1 .

[0029] (1) Solvent extraction: Weigh 20 g dry sample powder of Ou mandarin fruit oil cell layer, and use 400 mL of 80% ethanol (solid-to-liquid ratio 1:20) to sonicate for 40 min (ultrasonic frequency 60 kHz, power 30 W), the extract Centrifuge at 4000 rpm for 10 min on a centrifuge, repeat this twice, combine the supernatant, evaporate to dryness on a rotary evaporator to an ethanol-free phase, dissolve in about 200 mL of water, and use n-hexane, chloroform, n- Butanol was extracted twice (about 200 mL each time, 4 h each time), and the two extracts were combined respectively to obtain n-hexane extract, chloroform extract and n-butanol extract, and each extract was dissolved by rotary evaporation. In methanol, the flavonoid components of each fraction were de...

Embodiment 3

[0035] The method for the separation and purification of flavonoids in the oil cell layer of Ou mandarin orange according to the present invention is carried out according to the following three steps, see figure 1 .

[0036] (1) Solvent extraction: Weigh 100 g dry sample powder of Ou mandarin fruit oil cell layer, and use 2000 mL of 80% ethanol (solid-to-liquid ratio 1:20) to sonicate for 40 min (ultrasonic frequency 60 kHz, power 30 W). Centrifuge at 4000 rpm for 10 min on a centrifuge, repeat this twice, combine the supernatant, evaporate to dryness on a rotary evaporator to an ethanol-free phase, dissolve in about 800 mL of water, and use n-hexane, chloroform, n- Butanol was extracted twice (about 800 mL each time, 4 h each time), and the two extracts were combined respectively to obtain n-hexane extract, chloroform extract and n-butanol extract, and each extract was dissolved in In methanol, the flavonoid components of each fraction were determined by HPLC detection.

...

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Abstract

The invention provides a method for separating and purifying seven flavonoid compounds from a tangerine oil vacuole layer. According to the method provided by the invention, three steps, which are solvent extraction, Sephadex gel filtration and high-speed countercurrent chromatography (HSCCC) purification are adopted, a tangerine fruit oil vacuole layer is used as a raw material, seven flavonoid compounds can be obtained finally by virtue of purification, and the purities of the seven flavonoid compounds are over 97 percent. The method is simple in operation, short in production cycle, small in sample dosage and little in equipment investment, the condition is stable and easily controlled, and the seven flavonoid compounds comprise naringin, hesperidin, neohesperidin, sinensetin, nobiletin, tangeretin and 5-demethylnobiletin. The method is applicable to industrial production and scientific study.

Description

technical field [0001] The invention belongs to the technical field of extraction, separation and purification of active ingredients in natural plants, and specifically relates to the simultaneous separation and purification of Ou mandarin oranges by using the combination technology of solvent extraction, Sephadex gel filtration and high-speed countercurrent chromatography (HSCCC) using the Ou mandarin oil cell layer as a raw material Methods of seven flavonoids in the oleaginous layer. Background technique [0002] Ou Tangerine ( Citrus reticulata cv. Suavissima ) is a cultivar of Citrus genus of Rutaceae, a traditional specialty of Wenzhou, Zhejiang, with a cultivation history of more than two thousand years. Ou mandarin fruit has special curative effects such as anti-cancer, antipyretic and cooling, relieving phlegm and cough, cooling and detoxifying, improving blood circulation, and lowering blood pressure. These effects may be related to the flavonoids rich in its f...

Claims

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Application Information

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IPC IPC(8): A61K36/752
Inventor 李鲜张九凯孙崇德陈昆松
Owner ZHEJIANG UNIV
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