CN102491999A - Method for extracting polygonatum rhizome oligosaccharide - Google Patents

Abstract

The invention discloses a method for extracting polygonatum rhizome oligosaccharide, comprising the followings steps: carefully selecting raw materials, slicing, crushing, micro-grinding, carrying out reflux extraction, eluting through macroporous resin adsorption, carrying out active carbon column chromatography, carrying out gel column chromatography, and drying. The polygonatum rhizome oligosaccharide obtained by the method is gray white powder, and the sugar content is 90-93 %. According to the invention, the extraction is carried out under the condition of ultrafine particles, thus the extraction efficiency of the effective components is increased; the extraction process has no need of heating, thus the damage of high temperature to the effective components is avoided, the operation steps are simplified, and the purposed of increasing economic benefits is achieved.

Description

The process for extracting of sealwort oligose

Technical field

The present invention relates to a kind of sealwort oligose process for extracting, particularly a kind of method of from sealwort, extracting the sealwort oligose.

Background technology

Sealwort is a Liliaceae Polygonatum per nnial herb, and sealwort is arranged, Yunnan sealwort and David's-harp etc., and its dry rhizome is used as medicine.According to the classical record of traditional medicine, sealwort belongs to rare Chinese medicine, have wide in beneficial gas, enriching kidney essence, nourishing Yin and moistening lung, the effect of the tonifying spleen of promoting the production of body fluid.Cure mainly illnesss such as dryness of the lung dry cough, body void are weak, shortness of breath and palpitation, prolonged illness body fluid deficiency dry, mellitus, hypertension.To treatment cardiovascular disorder, white plaque, chronic hepatitis and at antibiotic, detoxifcation, antifatigue, anti-ageing, hypoglycemic, reducing blood-fat, aspect such as antitumor better effect is arranged all; Can be used as medicine; Can be used as protective foods again; Since ancient times, people as the good merchantable brand of promoting longevity, are sealwort tonic Chinese medicines commonly used.

In recent years, people deepen continuously to the Polygonatum Study on plants, from this platymiscium, have separated obtaining a lot of chemical ingredientss: polysaccharide, oligose, steroidal saponin, flavones etc.; Wherein oligose has different physiological roles; Mainly contain and suppress intracellular toxin, protection liver function, regulate gastrointestinal function, anti-treating constipation and diarrhoea, synthesise vitamins; Promote the absorption of mineral elements such as calcium, magnesium, zinc, iron; Reduce serum cholesterol, reduce fat and blood pressure, activate immunity, delay senility and effect such as antitumor, preventing dental caries, thereby being in great demand to the sealwort oligose.

To the extraction of sealwort oligose, generally adopt physics, chemical process, it is that the course of processing has high temperature that there is the problem of a maximum in these methods, causes the destruction to effective constituent easily.

The patent No. 2008100501457 discloses " from sealwort, extracting the sealwort oligose of raise immunity effect "; Extract the sealwort oligose with the ultrasonic alcohol extracting method that involves; Though this method can be extracted the sealwort oligose,, a lot of wastes have been caused because efficient is not high.

Summary of the invention

Technical problem to be solved by this invention provides a kind of method that adopts supersonic method from ultra-fine sealwort particle, to extract the sealwort oligose; With the extraction yield that improves the sealwort oligose, reduce destruction to the sealwort oligose; The step that simplifies the operation reaches the purpose of increasing economic efficiency.

For solving the problems of the technologies described above; The technical scheme that the present invention adopted is a kind of sealwort oligose process for extracting; Its technical process is that picking of raw material, section, pulverizing, micro mist are broken, refluxing extraction, concentrate, macroporous resin adsorption wash-out, activated carbon column chromatography, gel filtration chromatography, drying, concrete steps are following.

⑴ picking of raw material: the sealwort that is up to the standards is washed, dries.

⑵ section: the sealwort after will drying is thinly sliced, sheet thickness 0.3～0.7mm.

⑶ pulverize: the sealwort thin slice after will cutting is put into kibbler and is carried out just pulverizing, and powder particle diameter is 0.05～0.1mm.

⑷ micro mist is broken: the sealwort powder after will just pulverizing is put into pulverising mill and is pulverized, and powder particle diameter is 20～30um.

⑸ refluxing extraction: the ethanol that the sealwort powder is added 12 times of amounts 80%; Extracted 180 minutes 85 ℃ of water bath condition refluxed, filter, 80% ethanol that filter residue adds 10 times of amounts was 85 ℃ of water-bath refluxing extraction 120 minutes; Filter; 80% ethanol that filter residue adds 7 times of amounts filters 85 ℃ of water-bath refluxing extraction 60 minutes, merges filtrating three times.

⑹ concentrate: the rotary evaporation of will filtrate concentrates 10 times, liquid concentrator to the furnace pot 40 ℃ of water-baths wave most ethanol, must sealwort small molecular sugar position medicinal extract.

⑺ macroporous resin adsorption wash-out: with sealwort small molecular sugar position medicinal extract; With using macroporous resin adsorption behind the dissolved in distilled water again, hold over night is adsorbed impurity such as saponin(e, flavones resin as far as possible fully; Use the zero(ppm) water wash-out again; Flow velocity 1mL/min merges water elution position solution, again the rotary evaporation concentrating under reduced pressure.

⑻ activated carbon column chromatography: with activated carbon column on the liquid concentrator of water elution position, hold over night is fully adsorbed it, with zero(ppm) water, 10% ethanol, 20% ethanol gradient elution, remerges each several part elutriant and concentrating under reduced pressure.

⑼ gel filtration chromatography: liquid concentrator is used equal dissolved in distilled water, and last gel column carries out wash-out with zero(ppm) water under room temperature, and flow velocity is 0.5 mL/min, with the elutriant concentrating under reduced pressure.

⑽ dry: with liquid concentrator lyophilize 2 days in-80 ℃～-85 ℃ vacuum, the pearl loose powder occurs, promptly get the sealwort oligose.

The sealwort oligose that present method obtains is a pale powder, and sugar degree is 90～93%, and hydrolysising product analysis is for being monose, and dehydration forms furfural derivatives rapidly, is colored compound with the phenol condensation then, at the 490nm place characteristic absorbance is arranged.

The invention has the beneficial effects as follows that extracting whole process need not heating, has avoided the destruction of high temperature to effective constituent; Under ultrafine particulate, extract, improved extraction ratio of effective constituents.

Description of drawings

Accompanying drawing is a sealwort oligose process for extracting schema.

Embodiment

Below in conjunction with embodiment the present invention is described further.

Embodiment 1.

Get sealwort 10kg, clean, dry, be cut into the thin slice of thickness 0.5mm; The sealwort thin slice is put into kibbler carry out just pulverizing, powder particle diameter is 0.05～0.06mm; And then put into pulverising mill and pulverize again, powder particle diameter is 25～30um; Ethanol 120L with sealwort powder adding 80% extracted 180 minutes 85 ℃ of water bath condition refluxed, filtered; Filter residue adds 80% ethanol 100L again, 85 ℃ of water-bath refluxing extraction 120 minutes, filters; Filter residue adds 80% ethanol 70L; 85 ℃ of water-bath refluxing extraction 60 minutes, filter, merge filtrating three times; To filtrate concentrates 10 times with rotatory evaporator, in furnace pot, waves most ethanol with 40 ℃ of water-baths, obtains sealwort small molecular sugar position medicinal extract; With zero(ppm) water sealwort small molecular sugar position medicinal extract is dissolved then, use macroporous resin adsorption again, hold over night is used the zero(ppm) water wash-out again, and flow velocity 1mL/min merges water elution position solution, uses the rotatory evaporator concentrating under reduced pressure again; With activated carbon column on the liquid concentrator, hold over night is fully adsorbed it then, with zero(ppm) water, 10% ethanol, 20% ethanol gradient elution, remerges each several part elutriant and concentrating under reduced pressure; Again liquid concentrator is used equal dissolved in distilled water, last gel column carries out wash-out with zero(ppm) water under room temperature; Flow velocity is 0.5 mL/min; With the elutriant concentrating under reduced pressure and be placed in-82 ℃ of vacuum lyophilize 2 days, the pearl loose powder occurs then, promptly get the sealwort oligose.

Embodiment 2.

Get sealwort 15kg, clean, dry, be cut into the thin slice of thickness 0.3mm; The sealwort thin slice is put into kibbler carry out just pulverizing, powder particle diameter is 0.07～0.08mm; And then put into pulverising mill and pulverize again, powder particle diameter is 20～25um; Ethanol 180L with sealwort powder adding 80% extracted 180 minutes 85 ℃ of water bath condition refluxed, filtered; Filter residue adds 80% ethanol 150L again 85 ℃ of water-bath refluxing extraction 120 minutes; Filter, filter residue added 80% ethanol 105L, 85 ℃ of water-bath refluxing extraction 60 minutes; Filter, merge filtrating three times; To filtrate concentrates 10 times with rotatory evaporator, in furnace pot, waves most ethanol with 40 ℃ of water-baths, obtains sealwort small molecular sugar position medicinal extract; With zero(ppm) water sealwort small molecular sugar position medicinal extract is dissolved then, use macroporous resin adsorption again, hold over night is used the zero(ppm) water wash-out again, and flow velocity 1mL/min merges water elution position solution, uses the rotatory evaporator concentrating under reduced pressure again; With activated carbon column on the liquid concentrator, hold over night is fully adsorbed it then, with zero(ppm) water, 10% ethanol, 20% ethanol gradient elution, remerges each several part elutriant and concentrating under reduced pressure; Again liquid concentrator is used equal dissolved in distilled water, last gel column carries out wash-out with zero(ppm) water under room temperature; Flow velocity is 0.5 mL/min; With the elutriant concentrating under reduced pressure and be placed in-80 ℃ of vacuum lyophilize 2 days, the pearl loose powder occurs then, promptly get the sealwort oligose.

Claims (1)

1. the process for extracting of sealwort oligose is characterized in that concrete steps are following:

⑴ picking of raw material: the sealwort that is up to the standards is washed, dries;

⑵ section: the sealwort after will drying is thinly sliced, sheet thickness 0.3～0.7mm;

⑶ pulverize: the sealwort thin slice after will cutting is put into kibbler and is carried out just pulverizing, and powder particle diameter is 0.05～0.1mm;

⑷ micro mist is broken: the sealwort powder after will just pulverizing is put into pulverising mill and is pulverized, and powder particle diameter is 20～30um;

⑸ refluxing extraction: the ethanol that the sealwort powder is added 12 times of amounts 80%; Extracted 180 minutes 85 ℃ of water bath condition refluxed, filter, 80% ethanol that filter residue adds 10 times of amounts was 85 ℃ of water-bath refluxing extraction 120 minutes; Filter; 80% ethanol that filter residue adds 7 times of amounts filters 85 ℃ of water-bath refluxing extraction 60 minutes, merges filtrating three times;

⑹ concentrate: the rotary evaporation of will filtrate concentrates 10 times, liquid concentrator to the furnace pot 40 ℃ of water-baths wave most ethanol, must sealwort small molecular sugar position medicinal extract;

⑺ macroporous resin adsorption wash-out: with sealwort small molecular sugar position medicinal extract; With using macroporous resin adsorption behind the dissolved in distilled water again, hold over night is adsorbed impurity such as saponin(e, flavones resin as far as possible fully; Use the zero(ppm) water wash-out again; Flow velocity 1mL/min merges water elution position solution, again the rotary evaporation concentrating under reduced pressure;

⑻ activated carbon column chromatography: with activated carbon column on the liquid concentrator of water elution position, hold over night is fully adsorbed it, with zero(ppm) water, 10% ethanol, 20% ethanol gradient elution, remerges each several part elutriant and concentrating under reduced pressure;

⑼ gel filtration chromatography: liquid concentrator is used equal dissolved in distilled water, and last gel column carries out wash-out with zero(ppm) water under room temperature, and flow velocity is 0.5 mL/min, with the elutriant concentrating under reduced pressure;

⑽ dry: with liquid concentrator lyophilize 2 days in-80 ℃～-85 ℃ vacuum, the pearl loose powder occurs, promptly get the sealwort oligose.

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