CN101297874A - Technique for extracting high-content effective composition from white peony root - Google Patents

Abstract

The invention provides an extraction technology of high-content white paeony root active ingredients, comprising crude extraction, dissolution, purification and such steps, the crude extraction adopts alcohol-water solution for extraction and uses alcohol ester solution for extraction, a white paeony root crude extract is obtained by concentration and drying, the purification adopts a macroporous absorption resin to carry out absorption and separation; the technology of the invention can greatly improve the content of paeoniflorin to 60 percent to 90 percent, the process has simple operation and lower cost, and the resin can be repeatedly used, which is applicable to industrial production.

Description

A kind of extraction process of high-content effective composition from white peony root

Technical field:

The invention relates to a kind of technology of from Chinese crude drug, extracting Chinese medicinal ingredients, relate to extract in the medicine Radix Paeoniae Alba therefrom the extraction process of high-load active ingredient specifically.

Background technology:

The Chinese medicine Radix Paeoniae Alba is the dry root of ranunculaceae plant Radix Paeoniae, has the suppressing the hyperactive liver pain relieving, nourishing blood for regulating menstruation, astringing YIN to stop sweating effect; It is dizzy to be used to have a headache, hypochondriac pain, stomachache, limb pain twin, blood deficiency and yellow complexion, menoxenia, spontaneous perspiration, night sweat.Pharmacological research shows that the Radix Paeoniae Alba has effects such as spasmolysis and analgesia, immunomodulating, antiinflammatory.The main effective ingredient that contains in the Radix Paeoniae Alba is peoniflorin, lactone glucoside of Radix Paeoniae, oxypaeoniflorin, benzoylpaeoniflorin etc., and wherein paeoniflorin content is more, is one of its main effective ingredient.

China Patent No. ZL97101960 discloses a kind of extracting method, and this method adopts alcohol-aqueous solvent reflux, extract,, with alcohol-ester solution extraction, the technology of concentrate drying.Content of paeoniflorin generally can only reach 30%～50% in the Radix Paeoniae Alba extract that this technology is extracted, and content is lower, not too is fit to the pharmacy needs; China Patent No. ZL00121532 discloses and has used aluminium sesquioxide column chromatography purification Radix Paeoniae Alba total glucosides in a kind of preparation injection process, make its paeoniflorin content can reach 80%, but the not reproducible use of aluminium sesquioxide in the aluminium sesquioxide column chromatography, be not suitable for the requirement of industrialized great production, its cost is also high.

Summary of the invention:

Purpose of the present invention has just provided a kind of preparation technology of high-content effective composition from white peony root extract.

Concrete technology of the present invention is as follows:

1) slightly carry: the Radix Paeoniae Alba is put in the alcohol-water solution, and the concentration of alcohol is 40-95%, and weight ratio (W/V) is the Radix Paeoniae Alba: alcohol=1: 1-10, reflux 0.5-5 hour, filter, concentrate, filtrate transfers to P H-number 3-9 with diluted alkaline, the mixed liquor extraction of the pure and mild ester of reuse three times, the ratio of alcohol ester (V/V) is 5-80%, combining extraction liquid, concentrating under reduced pressure, drying gets Radix Paeoniae Alba crude extract.

Alcohol in alcohol in the said method-water liquid can be: methanol, ethanol, isopropyl alcohol, and a kind of in the propanol, used alkali can be: NaHCO ₃, NaOH, KHCO ₃, KOH's is a kind of, and the mixed liquor of pure and mild ester can be: methanol-ethyl acetate, ethanol-ethyl acetate, propanol-ethyl acetate, butanols-ethyl acetate a kind of, extraction temperature is 0-75 ℃.

2) dissolving is made aqueous solution or little suspendible shape solution with Radix Paeoniae Alba crude extract with hydrophilic solvent dissolving and filtration, and adjusting pH value with diluted alkaline is 4～9.

Described hydrophilic solvent can be one or several mixed solvents in methanol, ethanol, propanol, isopropyl alcohol, the acetone; Used alkali can be: NaHCO ₃, NaOH, KHCO ₃, a kind of among the KOH, the consumption of described hydrophilic solvent is 1～50 times of Radix Paeoniae Alba crude extract weight.

3) purification adopts macroporous adsorbent resin that aqueous solution is adsorbed, be adsorbed to saturated after, wash decontamination earlier with water to the Molish reaction negative, 1～10 times of amount of resin of the hydrophilic solvent of 20%～90% final concentration of 2～20 times of amount of resin of reuse/hour flow velocity (V/H) eluting target substance, eluent decompression backwater solvent, vacuum drying or spray drying are made the Radix Paeoniae Alba total glucosides extract.

Described macroporous adsorbent resin can be HPD-100, HPD-300, HPD-400, HPD-500, HPD-600, the HPD-700 of polystyrene skeleton, among the HPD-800 one or more; Also can be D101, the DK110 of polyacrylic acid skeleton, among the DK113 one or more.

Macroporous adsorbent resin is a kind of polymer absorbant with porous three dimensional structure synthetic, it is a class new type resin that on ion-exchanger and other adsorbent application foundation, grows up, be the Van der Waals force that relies between it and the molecule (adsorbate) that is adsorbed, undertaken by its huge specific surface that physical absorption works.In actual applications to some molecules close such as the very strong absorbability of the outstanding tool of aromatic series ring-type chemical compound with its framing structure.The present invention has improved content of paeoniflorin greatly owing to adopted the macroporous resin adsorption isolation technics, reaches 60%～90%, and this technological operation is easy, and cost is lower, and resin can use repeatedly, is fit to commercial production.

The used content assaying method of the present invention is the high effective liquid chromatography for measuring paeoniflorin content: chromatographic condition is for being filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.1% phosphoric acid solution (14: 86) is mobile phase; The detection wavelength is 230nm; Reference substance is a peoniflorin.Number of theoretical plate calculates by the peoniflorin peak should be not less than 2000.

The specific embodiment:

Embodiment 1

The ethanol-water solution of 300ML50% is added in the 100G Radix Paeoniae Alba, and reflux 1 hour is filtered, and concentrates, and uses rare NaHCO ₃Solution is regulated PH=8, and with 30ML20% ethanol-ethyl acetate, extraction is 3 times under 5 degree temperature, combining extraction liquid, concentrating under reduced pressure, vacuum drying, get Radix Paeoniae Alba crude extract, the hydrophilic solvent ethanol of gained Radix Paeoniae Alba crude extract being put into 10 times of its weight dissolves, and uses diluted alkaline NaHCO ₃Adjusting pH value is 4, adopt the HPD-100 macroporous adsorbent resin of polystyrene skeleton that aqueous solution is adsorbed, be adsorbed to saturated after, wash decontamination earlier with water to the Molish reaction negative, 3 times of amount of resin of the hydrophilic solvent of 20%～90% final concentration of 5 times of amount of resin of reuse/hour flow velocity (V/H) eluting target substance, eluent decompression backwater solvent, vacuum drying or spray drying are made the Radix Paeoniae Alba total glucosides extract.

Embodiment 2

200ML40% methanol-water solution is added in the 100G Radix Paeoniae Alba, reflux 2 hours, filter, concentrate, regulate PH=9 with NaOH, extract three times under 10 temperature with 30ML40% methanol-acetic acid ethyl fluid, combining extraction liquid, concentrating under reduced pressure, vacuum concentration, vacuum drying, get Radix Paeoniae Alba crude extract, the hydrophilic solvent methanol of gained Radix Paeoniae Alba crude extract being put into 20 times of its weight dissolves, and adjusting pH value with diluted alkaline NaOH is 6, adopt the HPD-300 macroporous adsorbent resin of polystyrene skeleton that aqueous solution is adsorbed, be adsorbed to saturated after, wash decontamination earlier with water to Mol ish reaction negative, 5 times of amount of resin of the hydrophilic solvent of 20%～90% final concentration of 10 times of amount of resin of reuse/hour flow velocity (V/H) eluting target substance, eluent decompression backwater solvent, vacuum drying or spray drying are made the Radix Paeoniae Alba total glucosides extract.

Embodiment 3

150ML60% propanol-aqueous solution is added in the 100G Radix Paeoniae Alba, and reflux 3 hours is filtered, and concentrates, and uses rare KHCO ₃Solution is regulated PH=6, extracts three times combining extraction liquid with 30ML60% propanol-acetic acid ethyl fluid under 40 temperature, concentrating under reduced pressure, vacuum concentration, vacuum drying get the total crude extract of the Radix Paeoniae Alba, the hydrophilic solvent propanol of gained Radix Paeoniae Alba crude extract being put into 40 times of its weight dissolves, and uses diluted alkaline KHCO ₃Adjusting pH value is 9, adopt the D101 macroporous adsorbent resin of polyacrylic acid skeleton that aqueous solution is adsorbed, be adsorbed to saturated after, wash decontamination earlier with water to the Molish reaction negative, 10 times of amount of resin of the hydrophilic solvent of 20%～90% final concentration of 20 times of amount of resin of reuse/hour flow velocity (V/H) eluting target substance, eluent decompression backwater solvent, vacuum drying or spray drying are made the Radix Paeoniae Alba total glucosides extract.

Claims (1)

1, a kind of extraction process of high-content effective composition from white peony root, its concrete technology is as follows:

1) slightly carry: the Radix Paeoniae Alba is put in the alcohol-water solution, and the concentration of alcohol is 40-95%, and weight ratio (W/V) is the Radix Paeoniae Alba: alcohol=1: 1-10, reflux 0.5-5 hour, filter, concentrate, filtrate transfers to P H-number 3-9 with diluted alkaline, the mixed liquor extraction of the pure and mild ester of reuse three times, the ratio of alcohol ester (V/V) is 5-80%, combining extraction liquid, concentrating under reduced pressure, drying gets Radix Paeoniae Alba crude extract;

Alcohol in alcohol in the said method-water liquid can be: methanol, ethanol, isopropyl alcohol, and a kind of in the propanol, used alkali can be: NaHCO ₃, NaOH, KHCO ₃, KOH's is a kind of, and the mixed liquor of pure and mild ester can be: methanol-ethyl acetate, ethanol-ethyl acetate, propanol-ethyl acetate, butanols-ethyl acetate a kind of, extraction temperature is 0-75 ℃;

2) dissolving is made aqueous solution or little suspendible shape solution with Radix Paeoniae Alba crude extract with hydrophilic solvent dissolving and filtration, and adjusting pH value with diluted alkaline is 4～9;

Described hydrophilic solvent can be one or several mixed solvents in methanol, ethanol, propanol, isopropyl alcohol, the acetone; Used alkali can be: NaHCO ₃, NaOH, KHCO ₃, a kind of among the KOH, the consumption of described hydrophilic solvent is 1～50 times of Radix Paeoniae Alba crude extract weight;

3) purification adopts macroporous adsorbent resin that aqueous solution is adsorbed, be adsorbed to saturated after, wash decontamination earlier with water to the Molish reaction negative, 1～10 times of amount of resin of the hydrophilic solvent of 20%～90% final concentration of 2～20 times of amount of resin of reuse/hour flow velocity (V/H) eluting target substance, eluent decompression backwater solvent, vacuum drying or spray drying are made the Radix Paeoniae Alba total glucosides extract;

Described macroporous adsorbent resin can be HPD-100, HPD-300, HPD-400, HPD-500, HPD-600, the HPD-700 of polystyrene skeleton, among the HPD-800 one or more; Also can be D101, the DK110 of polyacrylic acid skeleton, among the DK113 one or more.