CN103027937A - Method for extracting general flavone from honeysuckle leaves - Google Patents

Abstract

The invention relates to a method for extracting general flavone from honeysuckle leaves, belonging to the field of extraction of Chinese medicaments. The method comprises the following steps of: screening crushed honeysuckle leaves which are dried in the shade through a 40-mesh sieve; adding petroleum ether according to a material-liquid ratio (g/mL) of 1:(10 to 30); uniformly mixing; decolorizing for 30 minutes; filtering by using filter paper; drying filter residues for later use; accurately weighing the filter residues; adding an ethanol aqueous solution of which the concentration is 75 to 85 percent according to a material-liquid ratio (g/mL) of 1:(25 to 40); uniformly mixing; extracting for 2 to 4 hours for 2 to 3 times at 75 to 85 DEG C; performing suction filtration; concentrating the filtrate; drying in a refrigerating machine to obtain an extract; dissolving the extract by using distilled water to obtain a solution of which the concentration is 35 to 45 mg/mL; passing the mixture through D101 macroporous adsorption resin; eluting the mixture by using an ethanol aqueous solution of which the concentration is 70 to 80 percent at room temperature, wherein the flow speed is 1.0 to 1.5 mL/min, and the dosage of an eluant is 3 to 4 times of the volume of wet resin; and concentrating the eluant, and drying in the refrigerating machine to obtain the general flavone of which the purity is 80 to 85 percent. The method is simple, convenient and feasible; by adopting the method, the dosage of the solvent is low, the pollution to the environment is little, and the yield and the purity are higher; the ethanol aqueous solution is used for extraction, and is low in price and cost; the requirement for the purification temperature is low; and the macroporous resin is simple to regenerate and can be used for many times.

Description

A kind of method of extracting the leaf of Flos Lonicerae total flavones

Technical field

The invention belongs to the Chinese medicine extraction field, relate to a kind of method of extracting the leaf of Flos Lonicerae total flavones.

Background technology

The leaf of Flos Lonicerae caprifoliaceae plant has the effects such as heat-clearing and toxic substances removing, wind-heat dissipating.Flos Lonicerae contains enriches flavones ingredient, and demonstrates stronger anti-inflammatory activity, and document shows that general flavone content in the leaf of Flos Lonicerae is 2.78 times in spending, and the flavone component that therefore effectively extracts leaf of Flos Lonicerae is significant.The main methods such as alcohol-water solvent extraction, diluted alkaline alcohol extraction, ultrasound wave and supercritical fluid extraction of using are extracted flavone compound in the medicinal plants at present.

According to the extracting method of the leaf of Flos Lonicerae total flavones of result for retrieval and pertinent literature pertinent literature report, the following deficiency of ubiquity:

1. organic solvent lixiviate, organic solvent extraction, yield is low, and price is high, and environmental pollution is heavy.

2. equipment is complicated, and investment is large, poor stability.

3. flavone extraction ratio and purity are low.

Summary of the invention

The invention reside in provide a kind of extract the leaf of Flos Lonicerae total flavones method, for the research and development of leaf of Flos Lonicerae total flavones facilitate.

For realizing purpose of the present invention, existing according to following technical scheme.

A kind of method of extracting the leaf of Flos Lonicerae total flavones is characterized in that this extracting method comprises such as following steps:

(1) raw material is processed: the leaf of Flos Lonicerae of pulverizing that dries in the shade is crossed 40 mesh sieves.

(2) decolouring: be 1: 10～30 to add petroleum ether according to solid-liquid ratio (g/mL), mixing, decolouring 30min decolours twice;

(3) extract: be 1: 25～40 to add 75～85% ethanol water according to solid-liquid ratio (g/L), mixing,

Extracted 2～4 hours at 75～85 ℃, extract 2-3 time;

(4) separate: sucking filtration, filtrate is concentrated ,-80 ℃ of dry 12h-24h of vacuum refrigerating machine;

(5) absorption: extract dissolved in distilled water 35-45mg/mL solution, cross the D101 macroporous adsorbent resin;

(6) the ethanol water eluting of desorbing: 70-80%, flow velocity 1.0-1.5mL/min, room temperature, the eluant consumption is 3-4 times of wet resin volume;

(7) drying: eluent is concentrated ,-80 ℃ of dry 12h-24h of vacuum refrigerating machine.

The above-mentioned first step requires the leaf of Flos Lonicerae of drying and crushing to cross 40 mesh sieves.

Above-mentioned second step is 1: 10～30 adding petroleum ether according to solid-liquid ratio (g/mL), mixing, and decolouring 30min decolours twice.

Above-mentioned the 3rd described solvent extraction of step is the ethanol water of 1: 25～40 addings 75～85% according to solid-liquid ratio (g/mL), and mixing extracted 2～4 hours at 75～85 ℃, extracted 2-3 time.

Above-mentioned the 4th step is dry, adopts the dry 12h-24h of-80 ℃ of vacuum refrigerating machines.

It is the D101 macroporous adsorbent resin that above-mentioned the 5th step adopts, extract dissolved in distilled water 35-45mg/mL solution upper prop.

Above-mentioned the 6th step desorbed solution of telling is the 70-80% ethanol water, flow velocity 1.0-1.5mL/min, and room temperature, the eluant consumption is 3-4 times of wet resin volume.-80 ℃ of vacuum refrigerating machine dryings, the time is 12h-24h.

The inventive method is simple and easy to do, and solvent load is few, and environmental pollution is little; Yield and purity are higher; The employing ethanol water extracts, and price is low, and cost is little; Cleansing temp requires low; Macroporous resin regeneration is simple, can repeatedly use.

The specific embodiment:

Example 1:

Accurately weighed the leaf of Flos Lonicerae comminuted powder that 40 orders dry in the shade and pulverize, solid-liquid ratio (g/mL) adds petroleum ether at 1: 10, mixing, and decolouring 30min, decolouring twice is filtered.Filtering residue volatilizes for subsequent use.Accurately weigh the filtering residue that volatilizes, add 75% ethanol water extraction, solid-liquid ratio (g/mL) is 1: 25, and extracting temperature is 75 ℃, 2 hours extraction times, extraction time 2 times.Merge extractive liquid,, sucking filtration, filtrate is concentrated ,-80 ℃ of dry 12h of vacuum refrigerating machine.It is 35-45mg/mL solution upper prop that dissolved in distilled water is configured to concentration, and the D101 macroporous absorption is fully adsorbed, and 70% ethanol flow velocity is resolved with 1.0mL/min speed under the room temperature, and the eluant consumption is 3 times of wet resin volumes.Desorbed solution is concentrated, and-80 ℃ of dry 12h of vacuum refrigerating machine obtain purity and be 81.6% leaf of Flos Lonicerae total flavones.

Example 2:

Accurately weighed the leaf of Flos Lonicerae comminuted powder that 40 orders dry in the shade and pulverize, solid-liquid ratio (g/mL) adds petroleum ether at 1: 30, mixing, and decolouring 30min, decolouring twice is filtered.Filtering residue volatilizes for subsequent use.Accurately weigh the filtering residue that volatilizes, add 85% ethanol water extraction, solid-liquid ratio (g/mL) is 1: 40, and extracting temperature is 85 ℃, 4 hours extraction times, extraction time 3 times.Merge extractive liquid,, sucking filtration, filtrate is concentrated ,-80 ℃ of dry 12h of vacuum refrigerating machine.It is 35-45mg/mL solution upper prop that dissolved in distilled water is configured to concentration, and the D101 macroporous absorption is fully adsorbed, and 75% ethanol flow velocity is resolved with 1.5mL/min speed under the room temperature, and the eluant consumption is 3 times of wet resin volumes.Desorbed solution is concentrated, and-80 ℃ of dry 12h of vacuum refrigerating machine obtain purity and be 83.7% leaf of Flos Lonicerae total flavones.

Claims (1)

1. method of extracting the leaf of Flos Lonicerae total flavones is characterized in that this extracting method comprises such as following steps:

(1) raw material is processed: the leaf of Flos Lonicerae of pulverizing that dries in the shade is crossed 40 mesh sieves;

(2) decolouring: be 1: 10～30 to add petroleum ether according to solid-liquid ratio (g/L), mixing, decolouring 30min decolours twice;

(3) extract: be 1: 25～40 to add 75～85% ethanol water according to solid-liquid ratio (g/mL), mixing extracted 2～4 hours at 75～85 ℃, extracted 2-3 time;

(4) separate: sucking filtration, filtrate is concentrated ,-80 ℃ of dry 12h-24h of vacuum refrigerating machine;

(5) absorption: extract dissolved in distilled water 35-45mg/mL solution, cross the D101 macroporous adsorbent resin;

(6) the ethanol water eluting of desorbing: 70-80%, flow velocity 1.0-1.5mL/min, room temperature, the eluant consumption is 3-4 times of wet resin volume;

(7) drying: eluent is concentrated ,-80 ℃ of dry 12h-24h of vacuum refrigerating machine.