CN106309513A - Rhizoma drynariae extract production technology - Google Patents

Rhizoma drynariae extract production technology Download PDF

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Publication number
CN106309513A
CN106309513A CN201510395775.8A CN201510395775A CN106309513A CN 106309513 A CN106309513 A CN 106309513A CN 201510395775 A CN201510395775 A CN 201510395775A CN 106309513 A CN106309513 A CN 106309513A
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rhizoma drynariae
production technology
decoction
processes
resin
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赵忠海
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Beijing Qihuang Pharmaceutical Manufacturing Co Ltd
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Beijing Qihuang Pharmaceutical Manufacturing Co Ltd
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Abstract

The invention provides a rhizoma drynariae extract production technology. The rhizoma drynariae extract production technology comprises decoction treatment, filtering treatment, resin adsorption treatment, water washing treatment, ethanol elution treatment, condensation treatment, drying treatment, crushing treatment and rhizoma drynariae extract extraction. The rhizoma drynariae extract production technology improves the existing rhizoma drynariae extract production technology, improves extract general flavone content and improves a rhizoma drynariae general flavone yield.

Description

A kind of production technology of Rhizoma Drynariae extract
Technical field
The present invention relates to field of medicaments, be specifically related to the production technology of a kind of Rhizoma Drynariae extract.
Background technology
Rhizoma Drynariae (Rhizoma Drynariae) refers to Polypodiaceae (Polypodiaceae S.F.Gary) Mongolian oak Herba pteridii latiusculi Drynaria (Bory) J.Sm. plant such as Mongolian oak Herba pteridii latiusculi (Drynaria fortunei (kunze) J.Sm., Qinling Mountains Mongolian oak Herba pteridii latiusculi D.baronii (chist) Diels, drynaria baronii Diels D.sinica Diels, Drynaria delavayi christ D.delavayi Chirst, and Davalliaceae Davallia (Davallia Sm.) plant Rhizoma Drynariae The rhizome of one or more plants of Davallia mariesii Moore ex Bak or herb.
Process of Total Flavonoids in Drynaria Fortunei has effect of the kidney invigorating, bone strengthening and pain relieving, is usually utilized to treat constitutional bone Matter is loosened and the symptom such as pelvic bone or extremities joint pain.Process of Total Flavonoids in Drynaria Fortunei is usually and extracts from Rhizoma Drynariae Out, and the productivity of the Process of Total Flavonoids in Drynaria Fortunei of current production technology is relatively low.
Summary of the invention
In view of above-mentioned deficiency, it is an object of the invention to provide the production technology of a kind of new Process of Total Flavonoids in Drynaria Fortunei.
Technical scheme is as follows:
The production technology of a kind of Rhizoma Drynariae extract, comprises the steps:
S100: decoction processes;Use water that Rhizoma Drynariae raw material carries out decoction process and obtain decocting medicinal liquid, wherein Water is 5~15: 1 with the mass fraction ratio of described Rhizoma Drynariae raw material, and decocting time is 0.5~1.5 hour;
S200: filtration treatment;The ceramic membrane that described decoction medicinal liquid uses 100~150 mesh carries out filtration treatment Obtain filtrate;
S300: resin absorption processes;Use macroporous adsorptive resins that described filtrate is carried out resin absorption process, The flow velocity of wherein said filtrate is 5~7L/ minute * 100kg resin, and in described macroporous adsorptive resins, macropore is inhaled Resin is 1.5~2.5: 1 with the mass fraction ratio of described Rhizoma Drynariae raw material;
S400: washing processes;After resin absorption has processed, described macroporous adsorptive resins is washed Process colourless to effluent;
S500: ethanol elution processes;Ethanol is used described macroporous adsorptive resins to be carried out eluting process and receives Collection eluting effluent obtains collecting liquid, and the flow velocity of ethanol is 1~3L/ minute * 100kg resin;
S600: concentration;Described collection liquid being carried out concentration and obtains thick paste, described thick paste is with described The relative density collecting liquid is 1.19~1.21: 1;
S700: dried;Described thick paste is carried out vacuum drying treatment and obtains Process of Total Flavonoids in Drynaria Fortunei intermediate; Temperature≤80 DEG C of described dried, vacuum≤-0.085MPa;
S800: pulverization process;Described Process of Total Flavonoids in Drynaria Fortunei intermediate carries out pulverization process obtain Rhizoma Drynariae and carry Take thing.
Further, decoction described in step S100 processes and carries out three times, and the temperature that decoction processes is 100 DEG C.
Further, within step S200, the pressure of filtration treatment is 0.4MPa.
Further, the flow velocity of water that in step S400, washing processes is 30~50L/ minute.
Further, described step S500 starts when eluting effluent becomes brownish red to collect until institute State eluting effluent become faint yellow or colourless and/or stop time concentration of alcohol is 3% collecting.
Further, the mass percent of the ethanol used in described step S500 is 70~72%.
Further, concentration described in step S600 is carried out under vacuum is 0.05~0.06MPa.
Further, by carrying out Rhizoma Drynariae crude drug cutting into slices or pulverization process obtains during described Rhizoma Drynariae raw material Arriving, wherein the thickness of the section of Rhizoma Drynariae crude drug is 1~2mm, or obtain through pulverization process The granularity of Rhizoma Drynariae raw material is less than or equal to 10 mesh.
Further, total flavones contained in the described Rhizoma Drynariae extract that step S800 obtains is with naringin Meter content is 60%~65%.
The invention has the beneficial effects as follows: the production technology of the Rhizoma Drynariae extract of the present invention is at existing Rhizoma Drynariae Improved on the basis of the production technology of extract, improve the content of total flavones in extract, improved The productivity of Process of Total Flavonoids in Drynaria Fortunei.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with being embodied as Example, is further elaborated to the present invention.
It should be noted that in the case of not conflicting, the embodiment in the present invention and the feature in embodiment Can be mutually combined.Instrument employed in embodiments of the invention is commercially available, and water is drinking water or pure Water purification.
The invention provides the production technology of a kind of Rhizoma Drynariae extract, comprise the steps:
S100: decoction processes;Use water that Rhizoma Drynariae raw material carries out decoction process and obtain decocting medicinal liquid, wherein Water is 5~15: 1 with the mass fraction ratio of described Rhizoma Drynariae raw material, and decocting time is 0.5~1.5 hour.
The decoction of step S100 processes and can carry out repeatedly, repeatedly decoction processes the decoction medicinal liquid obtained and closes Filter after and, or directly carry out filtering the medicinal liquid after then filtering every time after can also decocting and close And.Decoction for the first time begins to warm up after needing to soak 20~40 minutes before processing.
Concrete, step S100 comprises the steps:
S110: feedwater;Rhizoma Drynariae raw material is placed in extraction pot, opens inlet valve, according to production technology Add appropriate drinking water, begin to warm up after soaking 20~40 minutes;
S120: be heated to boiling;Open cooling tower and make circulating cooling water running;It is first turned on straight-through steam valve Door is heated to boiling with straight-through jet chimney, and controlling straight-through steam pressure is below 0.15MPa, and temperature shows Instrument is shown as 100 ± 2 DEG C;Observe that mixture is closed straight-through after seething with excitement completely by the visor of extraction pot simultaneously Steam valve;
S130: insulation;The straight-through heating valve of closedown is opened behind the door and is indirectly heated valve, uses indirect sandwich heating, Controlling steam pressure is below 0.2MPa, makes medicinal liquid keep fluidized state.The secondary produced in decoction process Steam keeps circulation in returning to extraction pot by cooling tower after being cooled down.Temperature retention time is 0.5~1.5 hour.Decoct After the time of boiling reaches Preset Time, steam off valve, open vent valve and liquid valve, open spray pump, The first medicinal liquid decoction gone out is squeezed into and is carried out filtration treatment in filter or the medicinal liquid that decoction gone out squeezes into One fluid reservoir is kept in;
S140: secondary decoction processes;Repeat step S110 to S130 and obtain the second medicinal liquid;
S150: three decoctions process;Repeat step S110 to S130 and obtain the 3rd medicinal liquid.
S200: filtration treatment;The ceramic membrane that described decoction medicinal liquid uses 100~150 mesh carries out filtration treatment Obtain filtrate.Ceramic membrane in this step is arranged in the filter.The pressure filtered in this step is at 0.4MPa Within.
Wherein step S200 concrete operation step is for filling it up with medicine liquid irrigation, opens the bottom valve of medicine liquid irrigation, feed Pump turnover valve, the stop valve of circulation side, remaining valve closing.Start charging pump in filter, add injecting medical liquid, Air in emptying filter, circulating pump uses variable frequency starting, and (using low frequency during startup, pump to be recycled is transported Row steadily after the most slowly promote frequency until rated frequency), open the infiltration side valve of ceramic membrane after operating steadily Door collects filtrate.
S300: resin absorption processes;Use macroporous adsorptive resins that described filtrate is carried out resin absorption process, The flow velocity of wherein said filtrate is 5~7L/ minute * 100kg resin, and in described macroporous adsorptive resins, macropore is inhaled Resin is 1.5~2.5: 1 with the mass fraction ratio of described Rhizoma Drynariae raw material.The macroporous absorption tree used in this step Fat is HPD-D macroporous adsorbent resin.
Wherein step S300 comprises the steps:
S310: dress post;60 mesh rustless steel mesh grids will be placed to avoid macropore bottom macroporous adsorptive resins Adsorbent resin runs off, and closes outlet valve, and is placed in advance in 50 liters of water;Put into macropore according to a certain percentage Adsorbent resin;General, a diameter of 700mm to 800mm of macroporous adsorptive resins, preferably 750mm.
S320: pretreatment;First with water, macroporous adsorbent resin is rinsed to opening after effluent is colourless without alcohol taste Beginning adsorption treatment;
S330: adsorption treatment;Open spray pump, open macroporous adsorptive resins liquid feed valve, open big simultaneously Macroporous adsorbent resin liquid outlet valve, controlling filtrate flow velocity is 5~7L/ minute * 100kg resin.
Through test, other preparation conditions are equal, when flow velocity is 5~finally obtains during 7L/ minute * 100kg resin Rhizoma Drynariae extract in the content of total flavones be 60%~65%, be 10~20L/ minute * 100kg with flow velocity In the Rhizoma Drynariae extract that resin obtains, the content of total flavones is 50~55% to compare, and improves containing of total flavones Amount, improves the rate of transform of total flavones.
S400: washing processes;After resin absorption has processed, described macroporous adsorptive resins is washed Process colourless to effluent.In this step, the flow velocity of water is 40L/ minute.It concretely comprises the following steps opens water intaking valve Door, extrudes the medicinal liquid of remaining on macroporous adsorptive resins, when effluent color from depth to shallow until colourless time Wash complete.Now need to retain 2cm liquid level on macroporous adsorptive resins and treat ethanol elution.Further, for Guarantee tapping flow rate, in water-washing process, available water is from bleeder valve backwash macroporous adsorbent resin.
S500: ethanol elution processes;Use mass percent be 70~72% ethanol to described macroporous absorption tree Fat post carries out eluting process and collects eluting effluent and obtain collecting liquid, and the flow velocity of ethanol is 1~3L/ minute * 100kg resin.
The concrete operation step of step S500 is for opening ethanol fluid reservoir tapping valve, by ethanol injection macropore In adsorption resin column, start eluting.When eluent starts, color is become pale yellow from colourless, when effluent becomes Start during brownish red to collect and become faint yellow or colourless to effluent from brownish red and/or time concentration of alcohol is 3% Stop collecting.Colourless reservation liquid level is entered with water flushing macroporous adsorbent resin standby for next time after collection.S600: Concentration;Described collection liquid is carried out concentration and obtains thick paste, the phase of described thick paste and described collection liquid It is 1.19~1.21: 1 to density.Concentration described in step S600 is under vacuum is 0.05~0.06MPa Carry out.
Step S600 comprises the steps:
S610: pre-concentration;Pre-concentration is carried out in concentration pan;Concrete operation step is for opening vacuum pump and medicine Liquid liquid feed valve, is evacuated to collection liquid in concentration pan, when the liquid level collecting liquid arrives the lower visor on concentration pan Closing liquid feed valve time at 1/2, open steam valve and cooling circulating water valve, controlling vacuum is 0.05~0.06MPa, supplement eluent when medicinal liquid evaporation reduces from liquid feed valve until collecting liquid and all pumping;
S620: reconcentration;After collection liquid all pumps, close heating chamber steam valve, circulation butterfly valve;Beat Open atmospheric valve and liquid feed valve, by whole for the medicinal liquid in concentration pan suction to vaporization chamber, open jacket steam and continue Concentrate until obtaining meeting the thick paste of technological requirement.
The segmentation of step S600 is carried out, and uses steam direct heating can improve pre-concentration effect in the pre-concentration stage Rate, and use jacket steam to carry out heating in the reconcentration stage and can control the cocnentration factor of thick paste.This step is adopted Carry out with pre-concentration and reconcentration segmentation, the concentration time can be saved, can well control pre-simultaneously The quality concentrated.The concentration stage all uses steam direct heating to be difficult to control at follow-up enriching stage The enrichment of thick paste, according to experiment under conditions of same amount of liquid medicine, used by the concentration in the present invention Time is the time all using steam direct heating 1.1 times, the qualification rate of the thick paste obtained is up to More than 99%, reduce operation easier simultaneously.
S700: dried;Described thick paste is carried out vacuum drying treatment and obtains Process of Total Flavonoids in Drynaria Fortunei intermediate; Temperature≤80 DEG C of described dried, vacuum≤-0.085MPa.The standard of dried in this step For moisture less than 3%.
S800: pulverization process;Described Process of Total Flavonoids in Drynaria Fortunei intermediate carries out pulverization process obtain Rhizoma Drynariae and carry Take thing.
It should be noted that step S700 and step S800 must be carried out in D level clean area.
Carrying out three times it is also preferred that the left decoction described in step S100 processes, the temperature that decoction processes is 100 DEG C.
It is also preferred that the left within step S200, the pressure of filtration treatment is 0.4MPa.
It is also preferred that the left the flow velocity of water that in step S400, washing processes is 30~50L/ minute.
It is also preferred that the left described step S500 starts when eluting effluent becomes brownish red collect until described Eluting effluent becomes faint yellow or colourless and/or stops time concentration of alcohol is 3% collecting.
It is also preferred that the left cut into slices by Rhizoma Drynariae crude drug is carried out during Rhizoma Drynariae raw material used in the present invention or Pulverization process obtains, and wherein the thickness of the section of Rhizoma Drynariae crude drug is 1~2mm, or through pulverizing Process the granularity of the Rhizoma Drynariae raw material obtained less than or equal to 10 mesh.
It is also preferred that the left total flavones contained in the described Rhizoma Drynariae extract that obtains of step S800 is in terms of naringin Content is 60%~65%.
Specific embodiment:
In test, reagent used, reagent are analytical pure, and water is dual distilled water.
Total flavones in extract qualitatively judges with tetrahydro boron potassium chromogenic reaction.With UV absorptiometry to always Flavone is quantitative.Quantitative to naringin by high performance liquid chromatography (HPLC).
Tetrahydro boron potassium chromogenic reaction: access test fluid about 5ml with small test tube, adds tetrahydro boron potassium about 5mg, Shaking up, salt adding acid number drips, and in cherry red or aubergine represents and there is flavanone kind composition, sensitivity is 55μg/ml.If do not shown cherry red or aubergine, then it it is negative reaction.
Ultraviolet spectrophotometry carries out assay to total flavones: according to Chinese Pharmacopoeia version in 2010 Ultraviolet spectrophotometry (annex VA) measures.
With HPLC, naringin carried out assay: according to one efficient liquid phase of Chinese Pharmacopoeia nineteen ninety-five version Chromatography (annex VID) is measured.
Embodiment one
S110: feedwater;Weigh 100 grams of Rhizoma Drynariae raw materials to be placed in extraction pot, open inlet valve, press Add appropriate water according to production technology, begin to warm up after soaking 40 minutes;Water and the quality of Rhizoma Drynariae raw material Portion rate is 5: 1;
S120: be heated to boiling;Open cooling tower and make circulating cooling water running;It is first turned on straight-through steam valve Door is heated to boiling with straight-through jet chimney, and controlling straight-through steam pressure is below 0.15MPa, and temperature shows Instrument is shown as 100 ± 2 DEG C;Observe that mixture is closed straight-through after seething with excitement completely by the visor of extraction pot simultaneously Steam valve;
S130: insulation;The straight-through heating valve of closedown is opened behind the door and is indirectly heated valve, uses indirect sandwich heating, Controlling steam pressure is below 0.2MPa, makes medicinal liquid keep fluidized state.The secondary produced in decoction process Steam keeps circulation in returning to extraction pot by cooling tower after being cooled down.Temperature retention time is 0.5 hour.During decoction Between reach Preset Time after, steam off valve, open vent valve and liquid valve, open spray pump, will decoct The first medicinal liquid cooked is squeezed into and is carried out filtration treatment in filter or the first storage squeezed into by the medicinal liquid that decoction gone out Flow container is kept in;
S140: secondary decoction processes;Repeat step S110 to S130 and obtain the second medicinal liquid;
S150: three decoctions process;Repeat step S110 to S130 and obtain the 3rd medicinal liquid.
S200: filtration treatment;Use the ceramic membrane of 100 mesh to carry out filtration treatment described decoction medicinal liquid to obtain Filtrate.Ceramic membrane in this step is arranged in the filter.In this step filter pressure 0.4MPa with In.
S300: resin absorption processes;Use macroporous adsorptive resins that described filtrate is carried out resin absorption process, The flow velocity of wherein said filtrate is 5L/ minute * 100kg resin, and in described macroporous adsorptive resins, macropore inhales tree Fat is 1.5: 1 with the mass fraction ratio of described Rhizoma Drynariae raw material.
S400: washing processes;After resin absorption has processed, described macroporous adsorptive resins is washed Process colourless to effluent.In this step, the flow velocity of water is 30L/ minute.
S500: ethanol elution processes;Use mass percent be 70~72% ethanol to described macroporous absorption tree Fat post carry out eluting process and collect eluting effluent obtain collect liquid, the flow velocity of ethanol is 1L/ minute * 100kg resin.
S600: concentration;Described collection liquid is carried out concentration and obtains thick paste;
S700: described thick paste is carried out vacuum drying treatment and obtains Process of Total Flavonoids in Drynaria Fortunei intermediate;Described dry Temperature≤80 DEG C processed, vacuum≤-0.085MPa;
S800: described Process of Total Flavonoids in Drynaria Fortunei intermediate is carried out pulverization process and obtains Rhizoma Drynariae extract.
Finally obtain Rhizoma Drynariae extract 1.95 grams.Gained sample ultraviolet spectrophotometry is surveyed its total flavones and is contained Amount, general flavone content 60.08%, HPLC method measures naringin content 37.5% and (accounts for total flavones 67.2%).
Embodiment two
S110: feedwater;Weigh 100 grams of Rhizoma Drynariae raw materials to be placed in extraction pot, open inlet valve, press Add appropriate water according to production technology, begin to warm up after soaking 30 minutes;Water and the quality of Rhizoma Drynariae raw material Portion rate is 10: 1;
S120: be heated to boiling;Open cooling tower and make circulating cooling water running;It is first turned on straight-through steam valve Door is heated to boiling with straight-through jet chimney, and controlling straight-through steam pressure is below 0.15MPa, and temperature shows Instrument is shown as 100 ± 2 DEG C;Observe that mixture is closed straight-through after seething with excitement completely by the visor of extraction pot simultaneously Steam valve;
S130: insulation;The straight-through heating valve of closedown is opened behind the door and is indirectly heated valve, uses indirect sandwich heating, Controlling steam pressure is below 0.2MPa, makes medicinal liquid keep fluidized state.The secondary produced in decoction process Steam keeps circulation in returning to extraction pot by cooling tower after being cooled down.Temperature retention time is 0.5 hour.During decoction Between reach Preset Time after, steam off valve, open vent valve and liquid valve, open spray pump, will decoct The first medicinal liquid cooked is squeezed into and is carried out filtration treatment in filter or the first storage squeezed into by the medicinal liquid that decoction gone out Flow container is kept in;
S140: secondary decoction processes;Repeat step S110 to S130 and obtain the second medicinal liquid;
S150: three decoctions process;Repeat step S110 to S130 and obtain the 3rd medicinal liquid.
S200: filtration treatment;Use the ceramic membrane of 120 mesh to carry out filtration treatment described decoction medicinal liquid to obtain Filtrate.Ceramic membrane in this step is arranged in the filter.In this step filter pressure 0.4MPa with In.
S300: resin absorption processes;Use macroporous adsorptive resins that described filtrate is carried out resin absorption process, The flow velocity of wherein said filtrate is 6L/ minute * 100kg resin, and in described macroporous adsorptive resins, macropore inhales tree Fat is 2: 1 with the mass fraction ratio of described Rhizoma Drynariae raw material.
S400: washing processes;After resin absorption has processed, described macroporous adsorptive resins is washed Process colourless to effluent.In this step, the flow velocity of water is 40L/ minute.
S500: ethanol elution processes;Use mass percent be 70~72% ethanol to described macroporous absorption tree Fat post carry out eluting process and collect eluting effluent obtain collect liquid, the flow velocity of ethanol is 3L/ minute * 100kg resin.
S600: concentration;Described collection liquid is carried out concentration and obtains thick paste;
S700: described thick paste is carried out vacuum drying treatment and obtains Process of Total Flavonoids in Drynaria Fortunei intermediate;Described dry Temperature≤80 DEG C processed, vacuum≤-0.085MPa;
S800: described Process of Total Flavonoids in Drynaria Fortunei intermediate is carried out pulverization process and obtains Rhizoma Drynariae extract.
Finally obtain Rhizoma Drynariae extract 1.98 grams.Gained sample ultraviolet spectrophotometry is surveyed its total flavones and is contained Amount, general flavone content 64.08%, HPLC method measures naringin content 37.7% and (accounts for total flavones 67.1%).
Embodiment three
S110: feedwater;Rhizoma Drynariae raw material is placed in extraction pot, opens inlet valve, according to production technology Add appropriate water, begin to warm up after soaking 20 minutes;Water is 15: 1 with the mass fraction ratio of Rhizoma Drynariae raw material;
S120: be heated to boiling;Open cooling tower and make circulating cooling water running;It is first turned on straight-through steam valve Door is heated to boiling with straight-through jet chimney, and controlling straight-through steam pressure is below 0.15MPa, and temperature shows Instrument is shown as 100 ± 2 DEG C;Observe that mixture is closed straight-through after seething with excitement completely by the visor of extraction pot simultaneously Steam valve;
S130: insulation;The straight-through heating valve of closedown is opened behind the door and is indirectly heated valve, uses indirect sandwich heating, Controlling steam pressure is below 0.2MPa, makes medicinal liquid keep fluidized state.The secondary produced in decoction process Steam keeps circulation in returning to extraction pot by cooling tower after being cooled down.Temperature retention time is 0.5 hour.During decoction Between reach Preset Time after, steam off valve, open vent valve and liquid valve, open spray pump, will decoct The first medicinal liquid cooked is squeezed into and is carried out filtration treatment in filter or the first storage squeezed into by the medicinal liquid that decoction gone out Flow container is kept in;
S140: secondary decoction processes;Repeat step S110 to S130 and obtain the second medicinal liquid;
S150: three decoctions process;Repeat step S110 to S130 and obtain the 3rd medicinal liquid.
S200: filtration treatment;Use the ceramic membrane of 100 mesh to carry out filtration treatment described decoction medicinal liquid to obtain Filtrate.Ceramic membrane in this step is arranged in the filter.In this step filter pressure 0.4MPa with In.
S300: resin absorption processes;Use macroporous adsorptive resins that described filtrate is carried out resin absorption process, The flow velocity of wherein said filtrate is 7L/ minute * 100kg resin, and in described macroporous adsorptive resins, macropore inhales tree Fat is 2.5: 1 with the mass fraction ratio of described Rhizoma Drynariae raw material.
S400: washing processes;After resin absorption has processed, described macroporous adsorptive resins is washed Process colourless to effluent.In this step, the flow velocity of water is 20L/ minute.
S500: ethanol elution processes;Use mass percent be 70~72% ethanol to described macroporous absorption tree Fat post carry out eluting process and collect eluting effluent obtain collect liquid, the flow velocity of ethanol is 2L/ minute * 100kg resin.
S600: concentration;Described collection liquid is carried out concentration and obtains thick paste;
S700: described thick paste is carried out vacuum drying treatment and obtains Process of Total Flavonoids in Drynaria Fortunei intermediate;Described dry Temperature≤80 DEG C processed, vacuum≤-0.085MPa;
S800: described Process of Total Flavonoids in Drynaria Fortunei intermediate is carried out pulverization process and obtains Rhizoma Drynariae extract.
Finally obtain Rhizoma Drynariae extract 1.99 grams.Gained sample ultraviolet spectrophotometry is surveyed its total flavones and is contained Amount, general flavone content 65.01%, HPLC method measures naringin content 38.5% and (accounts for total flavones 68.2%).
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more concrete and detailed Carefully, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that, for this For the those of ordinary skill in field, without departing from the inventive concept of the premise, it is also possible to make some changes Shape and improvement, these broadly fall into protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be with Claim is as the criterion.

Claims (9)

1. the production technology of a Rhizoma Drynariae extract, it is characterised in that comprise the steps:
S100: decoction processes;Use water that Rhizoma Drynariae raw material carries out decoction process and obtain decocting medicinal liquid, wherein Water is 5~15: 1 with the mass fraction ratio of described Rhizoma Drynariae raw material, and decocting time is 0.5~1.5 hour;
S200: filtration treatment;The ceramic membrane that described decoction medicinal liquid uses 100~150 mesh carries out filtration treatment Obtain filtrate;
S300: resin absorption processes;Use macroporous adsorptive resins that described filtrate is carried out resin absorption process, The flow velocity of wherein said filtrate is 5~7L/ minute * 100kg resin, and in described macroporous adsorptive resins, macropore is inhaled Resin is 1.5~2.5: 1 with the mass fraction ratio of described Rhizoma Drynariae raw material;
S400: washing processes;After resin absorption has processed, described macroporous adsorptive resins is washed Process colourless to effluent;
S500: ethanol elution processes;Ethanol is used described macroporous adsorptive resins to be carried out eluting process and receives Collection eluting effluent obtains collecting liquid, and the flow velocity of ethanol is 1~3L/ minute * 100kg resin;
S600: concentration;Described collection liquid being carried out concentration and obtains thick paste, described thick paste is with described The relative density collecting liquid is 1.19~1.21: 1;
S700: dried;Described thick paste is carried out vacuum drying treatment and obtains Process of Total Flavonoids in Drynaria Fortunei intermediate; Temperature≤80 DEG C of described dried, vacuum≤-0.085MPa;
S800: pulverization process;Described Process of Total Flavonoids in Drynaria Fortunei intermediate carries out pulverization process obtain Rhizoma Drynariae and carry Take thing.
Production technology the most according to claim 1, it is characterised in that decoct described in step S100 Process is carried out three times, and the temperature that decoction processes is 100 DEG C.
Production technology the most according to claim 1, it is characterised in that filtration treatment in step S200 Pressure be 0.4MPa within.
Production technology the most according to claim 1, it is characterised in that in step S400, washing processes The flow velocity of water be 30~50L/ minute.
Production technology the most according to claim 1, it is characterised in that when washing in described step S500 De-effluent starts when becoming brownish red to collect until described eluting effluent becomes faint yellow or colourless and/or second Stop when determining alcohol is 3% collecting.
Production technology the most according to claim 1, it is characterised in that use in described step S500 The mass percent of ethanol be 70~72%.
Production technology the most according to claim 1, it is characterised in that concentrate described in step S600 Process and carry out under vacuum is 0.05~0.06MPa.
Production technology the most according to claim 1, it is characterised in that pass through during described Rhizoma Drynariae raw material Carry out Rhizoma Drynariae crude drug cutting into slices or pulverization process obtains, the wherein thickness of the section of Rhizoma Drynariae crude drug It is 1~2mm, or the granularity of the Rhizoma Drynariae raw material obtained through pulverization process is less than or equal to 10 mesh.
Production technology the most according to claim 1, it is characterised in that it is described that step S800 obtains Total flavones content in terms of naringin contained in Rhizoma Drynariae extract is 60%~65%.
CN201510395775.8A 2015-07-08 2015-07-08 Rhizoma drynariae extract production technology Pending CN106309513A (en)

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