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Orientin and homoorientin preparation method

A technology of isoorientin and orientin, which is applied in the field of separation and preparation of orientin and isoorientin, can solve the problems of low purity and long time, and achieve the effect of simplified process technology and easy control

Active Publication Date: 2015-02-25
江苏汉邦科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a method for the large-scale separation and preparation of orientin and isoorientin. The technical idea is to use a dynamic axial compression column for large-scale separation and preparation of orientin according to the principle of reversed-phase high-performance liquid chromatography. Glycoside and isoorientin solve the technical problems of long time and low purity existing in the process of purifying orientin and isoorientin at present. The operation is simple, the product content is high, and the reproducibility is good. The method includes the following step:

Method used

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  • Orientin and homoorientin preparation method
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  • Orientin and homoorientin preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0013] 1. Take 1g of crude bamboo leaf extract and dissolve it in water to make a saturated solution, treat it with ultrasound, filter to remove solid particles, and collect the filtrate for later use.

[0014] 2. Pump the filtrate from step 1 into the dynamic axial compression column preparation chromatography system, the column packing size is Φ50×250mm, the filler is octadecylsilane bonded silica gel, the particle size is 30um, and the sample volume is 1g , 0 to 40 minutes, the volume ratio of acetonitrile / water is from 20:80 to 40:60, the detection wavelength of the ultraviolet-visible photometric detector is 330nm, and the fraction of isoorientin with a retention time of 16~19min is collected, and the fraction of isoorientin is collected at 20~23min For the fraction of glucoside, after the elution of orientin and isoorientin is completed, the mobile phase is switched to acetonitrile with a high proportion to flush out the rear-end impurities, and a separation cycle ends. ...

Embodiment 2

[0016] 1. Take 2g of the crude bamboo leaf extract and dissolve it in water, prepare a saturated solution, treat it with ultrasound, filter to remove solid particles, and collect the filtrate for later use.

[0017] 2. Pump the filtrate from step 1 into the dynamic axial compression column preparation chromatography system, the column packing size is Φ50×250mm, the filler is octadecylsilane bonded silica gel, the particle size is 45um, and the loading volume is 2g , 0 to 40 minutes, the volume ratio of acetonitrile / water is from 25:75 to 50:50, the detection wavelength of the ultraviolet-visible photometric detector is 330nm, and the fraction of isoorientin with a retention time of 15-20min is collected, and the fraction of orientin is collected at 21-24min For the fraction of glucoside, after the elution of orientin and isoorientin is completed, the mobile phase is switched to acetonitrile with a high proportion to flush out the rear-end impurities, and a separation cycle ends...

Embodiment 3

[0019] 1. Take 10g of the crude bamboo leaf extract and dissolve it in water, prepare a saturated solution, ultrasonically treat, filter to remove solid particles, and collect the filtrate for later use.

[0020] 2. Pump the filtrate from step 1 into the dynamic axial compression column preparation chromatography system, the column packing size is Φ150×250mm, the filler is octadecylsilane bonded silica gel, the particle size is 70um, and the loading volume is 10g , 0 to 40 minutes, the volume ratio of acetonitrile / water is from 20:80 to 50:50, the detection wavelength of the ultraviolet-visible photometric detector is 330nm, and the fraction of isoorientin with a retention time of 16-21min is collected, and the fraction of orientin is collected at 22-25min For the fraction of glucoside, after the elution of orientin and isoorientin is completed, the mobile phase is switched to acetonitrile with a high proportion to flush out the rear-end impurities, and a separation cycle ends....

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Abstract

The invention relates to a method for separating preparation of carbon-glycoside flavonoid isomers, and particularly relates to a large-scale separation preparation method of orientin and homoorientin by a dynamic axial compression column, and the carbon-glycoside flavonoid isomers are extracted from bamboo leaves. The method solves the problems of low yield, high cost, long production cycle and the like of traditional separating preparation of the carbon-glycoside flavonoid isomers, and includes the following steps: 1) a bamboo leaf extract crude product is dissolved in water for ultrasonic treatment and filtration by a filter membrane, and the filtrate is taken for stand-by use; 2) the filtered crude product is separated and purified by a preparative liquid chromatography system; 3) solvents in elution solutions in corresponding bands are evaporated to obtain orientin and isoorientin monomers with the chromatographical purity of 98.5%. The separation and purification method is suitable for industrial separating preparation of the carbon-glycoside flavonoid isomers.

Description

technical field [0001] The invention relates to a method for the large-scale separation and preparation of carbon glycoside flavonoid isomers, in particular to a method for the separation and preparation of orientin and isoorientin. Background technique [0002] Orientin and its isomer isorientin, which belong to flavonoid glycosides, are easily soluble in water and ethanol, but insoluble in benzene, chloroform, ether and other organic solvents, and are the main components of bamboo leaf flavonoids. It has obvious biological and physiological activities such as anti-ulcer, antispasmodic, antibacterial, anti-inflammatory, hypolipidemic, analgesic and estrogen. Bamboo leaves have a long history of medicinal use in my country, and are blindly a famous heat-clearing and detoxifying medicine. The functional factors of bamboo leaf extract are mainly flavonoid glycosides. Bamboo leaf flavonoids have various biological activities, such as anti-lipid peroxidation, anti-aging, scaven...

Claims

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Application Information

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IPC IPC(8): C07D407/04
CPCC07D407/04
Inventor 张宇张大兵李胜迎
Owner 江苏汉邦科技股份有限公司