CN101766667A - Echinacea purpurea extract and preparing method and phenols ingredient detection method thereof - Google Patents
Echinacea purpurea extract and preparing method and phenols ingredient detection method thereof Download PDFInfo
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Abstract
The present invention discloses an echinacea purpurea extract. The echinacea purpurea extract comprises 2.4 to 3.1% of caftaric acid, 4.4 to 5.7% of chicoric acid and 1.5 to 2.0% of echinacoside based on the weight percentages of all ingredients accounting for the dry weight of the extract. The present invention also discloses a preparing method of echinacea purpurea extract and a detection method for phenols ingredient content in echinacea purpurea extract. The phenols ingredient content in the echinacea purpurea extract all meet the requirements of the active ingredient content specification of echinacea purpurea in United State Pharmacopeia 30 (USP 30). The phenols ingredient content is increased by 4 to 6% than that of echinacea purpurea extract sold on market. The preparing method has the advantages of simple technique, low cost, low energy consumption and easy industrialization.
Description
Technical field
The present invention relates to a kind of plant extract and its preparation method and reach the wherein detection method of composition, be specifically related to the detection method of content of a kind of Echinacea extract and its preparation method and phenols component thereof.
Background technology
Echinacea is a Compositae genus echinacea medicinal plants, originates in America, and China has some areas to introduce a fine variety, and medicinal part is root and rhizome or Herb.Echinacea has immunoloregulation function widely, can obviously improve the immunomodulating level of body, be mainly used in treatment flu (upper respiratory tract infection), typhoid fever, diphtheria, pulmonary tuberculosis and root bacterial infection disease of multiple florescence such as insecticide, venom, Echinacea also has antioxidation and antitumaous effect in addition.The genus echinacea plant main component comprise three major types, polysaccharide, caffeic acid derivant (mainly being chicoric acid, echinacoside, caffeoyl tartaric acid etc.) and alkyl amide compound.Echinacea all records at American Pharmacopeia (USP24-30 version), and the kind that American Pharmacopeia records comprises Echinacea medical material, Echinacea powder and Echinacea extract powder.At present, the product of Echinacea extract mainly contains 4% total phenols extract (UV method mensuration), 4% total phenols extract (HPLC method mensuration), 4% chicoric acid extract (HPLC method mensuration) on the domestic market, and wherein 4% total phenols extract is the main exit product.
Domestic patent about Echinacea extract has 4, now be exemplified below, publication number is the patent of CN1587251A: this patent is raw material with the Echinacea, prepares Echinacea extract through technical processs such as ethanol water extraction, diluted acid acidify, ethyl acetate extraction, macroporous resin separation, crystallisation by cooling.Because use organic solvents such as ethyl acetate in its preparation process, this extract has edible safety hidden danger; Publication number is the patent of CN1473602A: this patent is mixed with the Echinacea medical material with 30% ethanol water and is carried out reflux, extract,, back recovery extracting solution refluxes, medicinal residues continue the alcohol reflux with 30%, merge 2 times extracting solution, use the filtering with microporous membrane of 0.45 μ m then, filtrate is vacuum drying again, obtains extract.The preparation technology of its chicoric acid concentrates for filtrate, separates obtaining chicoric acid mutually with preparative liquid.This method is because the production cost costliness is not suitable for suitability for industrialized production; Publication number is the patent of CN1957961A: this patent is a raw material with the fresh blade of Echinacea medical material, alabastrum, side shoot, carry out cold pressing earlier, squeezed the juice, squeeze the juice again and to carry out reflux, extract, with 70～95% alcoholic solution, the extracting solution reconcentration obtains Echinacea extract.This method has only been measured the content of chicoric acid at Echinacea extract, can not represent the material composition of Echinacea performance drug effect; Publication number is the patent of CN101032541A: this patent is with 40～70% ethanol water reflux, extract, Echinacea medical materials, reclaims filtrate, again with 10～30% ethanol water reflux, extract, medicinal residues, merge 2 times extracting solution, concentrate, drying obtains Echinacea extract.Owing to lack purification step, the content of possible phenols component does not meet the requirement of American Pharmacopeia (USP30) about Echinacea extract.
Summary of the invention
Technical problem to be solved by this invention is in order to have edible safety hidden danger, production cost expensive and be not suitable for the defective of suitability for industrialized production in the preparation method that overcomes existing Echinacea extract, and a kind of Echinacea extract and preparation method thereof is provided.The content of phenols component all meets in the American Pharmacopeia 30 editions (USP30) requirement about Echinacea active constituent content regulation in the Echinacea extract of the present invention, and compare with commercially available Echinacea extract, the content of phenols component high by 4%～6% (percentage by weight), and its preparation method technology is simple, cost is low, energy consumption is little, is easy to industrialization.
The present invention relates to a kind of Echinacea extract, it contains caffeoyl tartaric acid 2.4%～3.1%, chicoric acid 4.4%～5.7% and echinacoside 1.5%～2.0%, and above percentage ratio is the percentage by weight that each composition accounts for the extract dry weight.
Wherein, caffeoyl tartaric acid, chicoric acid and echinacoside are total phenols component, and the content of total phenols component is 8.3%～10.8%, and above percentage ratio is the percentage by weight that each composition accounts for the extract dry weight.
The invention further relates to the preparation method of above-mentioned Echinacea extract, it comprises the following step:
(1) extraction, concentrated and centrifugal: the Echinacea medical material is extracted with ethanol water, extracting solution is concentrated, centrifugal then, get supernatant;
(2) membrance separation: with the supernatant thin up of step (1) gained, dilute liquid medicine filters through organic membrane, ultrafilter membrane and NF membrane successively, and filtrate is Echinacea extract.
Wherein, in the step (1), described extraction, concentrate and centrifugation method and condition all can be the conventional method and the condition of this area, preferable methods and condition are as follows: described Echinacea medical material is preferable is the medical material after pulverizing, and preferable particle size is 40 orders; What the temperature of described extraction was preferable is 70 ℃～100 ℃; Better is reflux temperature; What the concentration of described ethanol water was preferable is percent by volume 10%～60%; The each consumption that extracts of described ethanol water is preferable is 8～12 times of Echinacea medical material weight; What the number of times of described extraction was preferable is 1～3 time, and what each time was preferable is 0.5～2 hour; It is described that to concentrate preferable be with 1/3 of extracting solution simmer down to original liquid volume; That described centrifugal rotation speed is preferable is 4000～5000r/min;
In the step (2), what described water was preferable is deionized water; The consumption of water is preferable is 2 times of supernatant volume; That the pore size filter of described organic membrane is preferable is 250～400nm, and what the material of organic membrane was preferable is the hydrophilic polyvinylidene fluoride; That the pore size filter of described ultrafilter membrane is preferable is 5～15nm, and what the material of ultrafilter membrane was preferable is the hydrophilic polyvinylidene fluoride; That the pore size filter of described NF membrane is preferable is 0.1～1nm, and what the material of NF membrane was preferable is polyamide; Described through organic membrane carry out filtering operating pressure preferable be 0～0.5Mpa, that better is 0.2Mpa; Described through ultrafilter membrane carry out filtering operating pressure preferable be 0～0.8Mpa, that better is 0.6Mpa; Described through NF membrane carry out filtering operating pressure preferable be 0～3Mpa, that better is 1.5Mpa; What the operative temperature when above-mentioned three kinds of films filter was preferable is 20 ℃～35 ℃;
In the step (2), described filter the back preferable also comprise the following step: collect the NF membrane filtrate filtered, this filtrate carried out drying, obtain the Echinacea extract powder; What described exsiccant method was preferable is spray drying.
In the preparation method of the present invention, but the optimum condition combination in any of above-mentioned each processing step promptly obtains each preferred embodiments of the present invention.
Among the present invention, the optimization procedure of the preparation method of described Echinacea extract is as follows:
(a) alcohol reflux: with Echinacea pulverizing medicinal materials to 40 order, add percent by volume 40%～60% ethanol water reflux, extract, 2 times, each consumption is 8～12 times of amounts of Echinacea medical material weight, and each time is 0.5～2 hour, merges 40%～60% ethanol extract; Residue adds 10%～20% ethanol water reflux, extract,, and consumption is that the 8-12 of Echinacea medical material weight doubly measures, and the time is 1 hour, merges 40%～60% ethanol extract and 10%～20% ethanol extract then;
(b) concentrate: the extracting solution of step (a) gained is concentrated into 1/3 of original liquid volume;
(c) centrifugal: the medicinal liquid of step (b) gained is centrifugal with 4000～5000r/min, get supernatant;
(d) membrance separation: get supernatant, adding is that 2 times deionized water of supernatant volume fully dilutes, and dilute liquid medicine is further purified through organic membrane, ultrafilter membrane and NF membrane successively, the filtrate after the collection nanofiltration; Adopt the piece-rate system of membrance separation to be: the pore size filter of organic membrane is 250～400nm, and the material of organic membrane is the hydrophilic polyvinylidene fluoride; The pore size filter of ultrafilter membrane is 5～15nm, and the material of ultrafilter membrane is the hydrophilic polyvinylidene fluoride; The pore size filter of described NF membrane is 0.1～1nm, and the material of NF membrane is a polyamide; It is 0～0.5Mpa that described process organic membrane carries out filtering operating pressure, and that better is 0.2Mpa; It is 0～0.8Mpa that described process ultrafilter membrane carries out filtering operating pressure, and that better is 0.6Mpa; It is 0～3Mpa that described process NF membrane is carried out filtering operating pressure, and that better is 1.5Mpa; Operative temperature when above-mentioned three kinds of films filter is 20～35 ℃;
(e) spray drying: carry out spray drying through the NF membrane filtrate filtered, obtain the Echinacea extract powder.
Among the present invention, described Echinacea medical material is preferable is selected from genus echinacea plant Echinacea (Echinacea purpurea), Echinacea angustifolia (Echinacea angustifolia) or white Echinacea (Echinacea pallida).
The invention further relates to the detection method of content of phenols component in the above-mentioned Echinacea extract, it comprises following condition: detect with efficient liquid-phase chromatography method; With the octadecylsilane chemically bonded silica is filler; With acetonitrile and volumetric concentration is that 0.1% phosphoric acid solution is that eluent carries out gradient elution, and actual conditions sees Table 1; The detection wavelength is 330nm, and column temperature is 35 ℃, and flow velocity is 1.5ml/min;
Table 1
With caffeoyl tartaric acid, echinacoside and chicoric acid is reference substance; Above percentage ratio is percent by volume.
In this detection method, the preparation of reference substance solution, the preparation of need testing solution, standard curve draw and assay all can be existing conventional method and condition, preferred following method and condition:
The preparation of reference substance solution: it is an amount of to get caffeoyl tartaric acid, echinacoside and chicoric acid reference substance respectively, and accurate the title decides, and adds percent by volume 70% ethanol and makes the solution that every 1ml contains 80 μ g, promptly;
The preparation of need testing solution: take by weighing the about 1g of Echinacea extract powder of the present invention, the accurate title, decide, and places the 50ml volumetric flask, adds percent by volume 70% ethanol 20ml, ultrasonic 5 minutes, cooling added percent by volume 70% ethanol and is settled to scale, shakes up, filter, get filtrate, get final product;
Standard curve is drawn: accurate respectively caffeoyl tartaric acid, echinacoside and chicoric acid reference substance solution 2,4,6,8,10,12, the 14 μ l injection chromatograph of liquid drawn, measure each chromatograph peak-to-peak area, (μ g) is abscissa with the reference substance sample size, the chromatographic peak peak area is a vertical coordinate, the drawing standard curve;
Assay: accurate each the 10 μ l of 3 batches of need testing solutions that draw, inject chromatograph of liquid, measure 20 minutes chromatogram peak areas, calculate content and get final product.
Except that specified otherwise, raw material that the present invention relates to and reagent are all commercially available to be got.
Positive progressive effect of the present invention is:
(1) content of phenols component all meets in the American Pharmacopeia 30 editions (USP30) requirement about Echinacea active constituent content regulation in the Echinacea extract of the present invention, and compare with commercially available Echinacea extract, the content of phenols component is high by 4%～6%, and its preparation method technology is simple, cost is low, energy consumption is little, is easy to industrialization.
(2) in the preparation method of Echinacea extract of the present invention, the utilization membrane separation technique is removed biomacromolecule in the extract such as protein, tannin, colloidal type chemical compound, effect is obvious, the response rate is higher, and utilization membrane separation purification Echinacea extract does not have damage to film, and back capable of washing is reused.
Description of drawings
Fig. 1 is the high-efficient liquid phase chromatogram of chicoric acid reference substance.
Fig. 2 is the high-efficient liquid phase chromatogram of caffeoyl tartaric acid reference substance.
Fig. 3 is the high-efficient liquid phase chromatogram of echinacoside reference substance.
The high-efficient liquid phase chromatogram of the Echinacea extract test sample that Fig. 4 makes for embodiment 6.
The specific embodiment
Further specify the present invention with embodiment below, but the present invention is not limited.
In following examples, the concentration of ethanol water is volumetric concentration.
The preparation of embodiment 1 Echinacea extract
Get the dry medical material 2kg of Echinacea herb, pulverizing is 40 orders, added 8 times of amount 40% ethanol water reflux, extract, 0.5 hour, inclining extracting solution, and residue adds 10 times of amount 10% ethanol water reflux, extract, 1 hour, merge whole extracting solution, be evaporated to 1/3 of original volume, with the centrifugal 10min of 4000r/min, inclining supernatant, add 2 times of supernatant volumes of deionized water dilutions, diluent filters by organic membrane earlier, membrane aperture 300nm, operating pressure 0.2MPa, 28 ℃ of operative temperatures, obtain organic membrane permeate 50L, the organic membrane permeate separates by ultrafilter membrane again, membrane aperture 10nm, operating pressure 0.6MPa obtains ultrafiltration membrane permeate liquid 41L.The ultrafilter membrane filtered solution carries out NF membrane again and concentrates operating pressure 1.5Mpa.Filtrate after the collection nanofiltration.Carry out spray drying through the NF membrane filtrate filtered, spray-dired parameter is: 180 ℃ of inlet air temperature, 102 ℃ of leaving air temps, flow velocity 3.2L/h, collect spray-dried powders, promptly get Echinacea extract, caffeoyl tartaric acid, echinacoside and chicoric acid content sum are 8.3%, it contains caffeoyl tartaric acid 2.4%, chicoric acid 4.4% and echinacoside 1.5%.
The preparation of embodiment 2 Echinacea extracts
Get the dry medical material 2kg of Echinacea herb, pulverizing is 40 orders, adds 10 times of amount 50% ethanol water reflux, extract, 3 times, each 0.5 hour, incline and extracting solution, residue adds 10 times of amount 10% ethanol water reflux, extract, 1 hour, merges whole extracting solution, is evaporated to 1/3 of original volume, with the centrifugal 10min of 4000r/min, inclining supernatant, adds 2 times of supernatant volumes of deionized water dilutions, and diluent filters by organic membrane earlier, membrane aperture 300nm, operating pressure 0.2MPa, 28 ℃ of operative temperatures obtain organic membrane permeate 50L, the organic membrane permeate separates by ultrafilter membrane again, membrane aperture 10nm, operating pressure 0.6MPa obtains ultrafiltration membrane permeate liquid 41L.The ultrafilter membrane filtered solution carries out NF membrane again and concentrates operating pressure 1.5Mpa.Filtrate after the collection nanofiltration.Carry out spray drying through the NF membrane filtrate filtered, spray-dired parameter is: 180 ℃ of inlet air temperature, 102 ℃ of leaving air temps, flow velocity 3.2L/h, collect spray-dried powders, promptly get Echinacea extract, caffeoyl tartaric acid, echinacoside and chicoric acid content sum are 9.1% in the mensuration Echinacea extract, it contains caffeoyl tartaric acid 2.6%, chicoric acid 4.9% and echinacoside 1.6%.
The preparation of embodiment 3 Echinacea extracts
Get the dry medical material 2kg of Echinacea herb, pulverizing is 40 orders, added 12 times of amount 50% ethanol water reflux, extract, 2 hours, inclining extracting solution, and residue adds 10 times of amount 10% ethanol water reflux, extract, 1 hour, merge whole extracting solution, be evaporated to 1/3 of original volume, with the centrifugal 10min of 4000r/min, inclining supernatant, add 2 times of supernatant volumes of deionized water dilutions, diluent filters by organic membrane earlier, membrane aperture 300nm, operating pressure 0.2MPa, 28 ℃ of operative temperatures, obtain organic membrane permeate 50L, the organic membrane permeate separates by ultrafilter membrane again, membrane aperture 10nm, operating pressure 0.6MPa obtains ultrafiltration membrane permeate liquid 41L.The ultrafilter membrane filtered solution carries out NF membrane again and concentrates operating pressure 1.5Mpa.Filtrate after the collection nanofiltration.Carry out spray drying through the NF membrane filtrate filtered, spray-dired parameter is: 180 ℃ of inlet air temperature, 102 ℃ of leaving air temps, flow velocity 3.2L/h, collect spray-dried powders, promptly get Echinacea extract, caffeoyl tartaric acid, echinacoside and chicoric acid content sum are 10.8%, it contains caffeoyl tartaric acid 3.1%, chicoric acid 5.7% and echinacoside 2.0%.
The preparation of embodiment 4 Echinacea extracts
Get the dry medical material 2kg of Echinacea herb, pulverizing is 40 orders, adds 12 times of amount 60% ethanol water reflux, extract, 2 times, each 0.5 hour, incline and extracting solution, residue adds 10 times of amount 10% ethanol water reflux, extract, 1 hour, merges whole extracting solution, is evaporated to 1/3 of original volume, with the centrifugal 10min of 4000r/min, inclining supernatant, adds 2 times of supernatant volumes of deionized water dilutions, and diluent filters by organic membrane earlier, membrane aperture 300nm, operating pressure 0.2MPa, 28 ℃ of operative temperatures obtain organic membrane permeate 50L, the organic membrane permeate separates by ultrafilter membrane again, membrane aperture 10nm, operating pressure 0.6MPa obtains ultrafiltration membrane permeate liquid 41L.The ultrafilter membrane filtered solution carries out NF membrane again and concentrates operating pressure 1.5Mpa.Filtrate after the collection nanofiltration.Carry out spray drying through the NF membrane filtrate filtered, spray-dired parameter is: 180 ℃ of inlet air temperature, 102 ℃ of leaving air temps, flow velocity 3.2L/h, collect spray-dried powders, promptly get Echinacea extract, caffeoyl tartaric acid, echinacoside and chicoric acid content sum are 8.8%, it contains caffeoyl tartaric acid 2.5%, chicoric acid 4.7% and echinacoside 1.6%.
The preparation of embodiment 5 Echinacea extracts
Get the dry medical material 2kg of Echinacea herb, pulverizing is 40 orders, added 12 times of amount 60% ethanol water reflux, extract, 2 hours, inclining extracting solution, and residue adds 10 times of amount 10% ethanol water reflux, extract, 1 hour, merge whole extracting solution, be evaporated to 1/3 of original volume, with the centrifugal 10min of 4000r/min, inclining supernatant, add 2 times of supernatant volumes of deionized water dilutions, diluent filters by organic membrane earlier, membrane aperture 300nm, operating pressure 0.2MPa, 28 ℃ of operative temperatures, obtain organic membrane permeate 50L, the organic membrane permeate separates by ultrafilter membrane again, membrane aperture 10nm, operating pressure 0.6MPa obtains ultrafiltration membrane permeate liquid 41L.The ultrafilter membrane filtered solution carries out NF membrane again and concentrates operating pressure 1.5Mpa.Filtrate after the collection nanofiltration.Carry out spray drying through the NF membrane filtrate filtered, spray-dired parameter is: 180 ℃ of inlet air temperature, 102 ℃ of leaving air temps, flow velocity 3.2L/h, collect spray-dried powders, promptly get Echinacea extract, caffeoyl tartaric acid, echinacoside and chicoric acid content sum are 10.2%, it contains caffeoyl tartaric acid 2.9%, chicoric acid 5.4% and echinacoside 1.8%.
The preparation of embodiment 6 Echinacea extracts
Get the dry medical material 2kg of Echinacea herb, pulverizing is 40 orders, added 10 times of amount 60% ethanol water reflux, extract, 2 hours, inclining extracting solution, and residue adds 10 times of amount 10% ethanol water reflux, extract, 1 hour, merge whole extracting solution, be evaporated to 1/3 of original volume,, emit supernatant with the centrifugal 10min of 4000r/min, add 2 times of supernatant volumes of deionized water dilutions, diluent filters by organic membrane earlier, membrane aperture 300nm, operating pressure 0.2MPa, 28 ℃ of operative temperatures, obtain organic membrane permeate 50L, the organic membrane permeate separates by ultrafilter membrane again, membrane aperture 10nm, operating pressure 0.6MPa obtains ultrafiltration membrane permeate liquid 41L.The ultrafilter membrane filtered solution carries out NF membrane again and concentrates operating pressure 1.5Mpa.Filtrate after the collection nanofiltration.Carry out spray drying through the NF membrane filtrate filtered, spray-dired parameter is: 180 ℃ of inlet air temperature, 102 ℃ of leaving air temps, flow velocity 3.2L/h, collect spray-dried powders, promptly get Echinacea extract, caffeoyl tartaric acid, echinacoside and chicoric acid content sum are 10.8%, it contains caffeoyl tartaric acid 3.1%, chicoric acid 5.7% and echinacoside 2.0%.
The preparation of embodiment 7 Echinacea extracts
Get the dry medical material 2kg of Echinacea herb, pulverizing is 40 orders, adding 8 times of amount 60% ethanol waters extracted 1 hour for 70 ℃, incline and extracting solution, residue adds 8 times of amount 20% ethanol water reflux, extract, 1 hour, merges whole extracting solution, is evaporated to 1/3 of original volume, with the centrifugal 10min of 5000r/min, emit supernatant, add 2 times of supernatant volumes of deionized water dilutions, diluent filters by organic membrane earlier, the material of organic membrane is the hydrophilic polyvinylidene fluoride, membrane aperture 250nm, operating pressure 0～0.2MPa, 20 ℃ of operative temperatures, obtain organic membrane permeate 50L, the organic membrane permeate separates by ultrafilter membrane again, and the material of ultrafilter membrane is the hydrophilic polyvinylidene fluoride, membrane aperture 5nm, operating pressure 0～0.3MPa obtains ultrafiltration membrane permeate liquid 41L.The ultrafilter membrane filtered solution carries out NF membrane again and concentrates, and the material of NF membrane is a polyamide, membrane aperture 0.1nm, operating pressure 0～0.3Mpa.Filtrate after the collection nanofiltration.Carry out spray drying through the NF membrane filtrate filtered, spray-dired parameter is: 180 ℃ of inlet air temperature, 102 ℃ of leaving air temps, flow velocity 3.2L/h, collect spray-dried powders, promptly get Echinacea extract, caffeoyl tartaric acid, echinacoside and chicoric acid content sum are 10.8%, it contains caffeoyl tartaric acid 3.1%, chicoric acid 5.7% and echinacoside 2.0%.
The preparation of embodiment 8 Echinacea extracts
Get the dry medical material 2kg of Echinacea herb, pulverizing is 40 orders, adding 12 times of amount 60% ethanol waters extracted 1 hour for 100 ℃, incline and extracting solution, residue adds 12 times of amount 15% ethanol water reflux, extract, 1 hour, merges whole extracting solution, is evaporated to 1/3 of original volume, with the centrifugal 10min of 4500r/min, emit supernatant, add 2 times of supernatant volumes of deionized water dilutions, diluent filters by organic membrane earlier, the material of organic membrane is the hydrophilic polyvinylidene fluoride, membrane aperture 400nm, operating pressure 0.5MPa, 35 ℃ of operative temperatures, obtain organic membrane permeate 50L, the organic membrane permeate separates by ultrafilter membrane again, and the material of ultrafilter membrane is the hydrophilic polyvinylidene fluoride, membrane aperture 15nm, operating pressure 0.8MPa obtains ultrafiltration membrane permeate liquid 41L.The ultrafilter membrane filtered solution carries out NF membrane again and concentrates, and the material of NF membrane is a polyamide, membrane aperture 1nm, operating pressure 3Mpa.Filtrate after the collection nanofiltration.Carry out spray drying through the NF membrane filtrate filtered, spray-dired parameter is: 180 ℃ of inlet air temperature, 102 ℃ of leaving air temps, flow velocity 3.2L/h, collect spray-dried powders, promptly get Echinacea extract, caffeoyl tartaric acid, echinacoside and chicoric acid content sum are 10.8%, it contains caffeoyl tartaric acid 3.1%, chicoric acid 5.7% and echinacoside 2.0%.
Equipment used in the present invention is the used common apparatus of chemical pharmaceutical industry, as membrane separation plant, centrifuge etc.
The detection of phenols component in embodiment 9 Echinacea extracts
The detection method of phenols component:
Efficient liquid-phase chromatography method detects, chromatographic condition is: be filler with the octadecylsilane chemically bonded silica, with acetonitrile～volumetric concentration is 0.1% phosphoric acid solution gradient elution, actual conditions sees Table 1, the detection wavelength is 330nm, column temperature is 35 ℃, and flow velocity is 1.5ml/min, and percentage ratio is percent by volume in the table.
Table 1
The preparation of reference substance solution: it is an amount of to get caffeoyl tartaric acid, echinacoside, chicoric acid reference substance respectively, accurately claims surely, adds 70% ethanol and makes the solution that every 1ml contains 80 μ g, promptly.
The preparation of need testing solution: take by weighing the about 1g of Echinacea extract powder that embodiments of the invention 6 make, the accurate title, decide, and places the 50ml volumetric flask, adds 70% ethanol 20ml, ultrasonic 5 minutes, cooling added 70% ethanol and is settled to scale, shakes up, filter, get subsequent filtrate, promptly.
Standard curve is drawn: accurate respectively absorption caffeoyl tartaric acid, echinacoside, chicoric acid reference substance solution 2,4,6,8,10,12,14 μ l inject chromatograph of liquid, measure each chromatograph peak-to-peak area, (μ g) is abscissa with the reference substance sample size, the chromatographic peak peak area is a vertical coordinate, the drawing standard curve.
Algoscopy: accurate each the 10 μ l of 3 batches of need testing solutions that draw, inject chromatograph of liquid, measure 20 minutes chromatogram peak areas, calculate content.
Reference substance and test sample chromatogram are seen accompanying drawing 1～4.
Claims (10)
1. Echinacea extract, it is characterized in that: it contains caffeoyl tartaric acid 2.4%～3.1%, chicoric acid 4.4%～5.7% and echinacoside 1.5%～2.0%, above percentage ratio is the percentage by weight that each composition accounts for the extract dry weight.
2. the preparation method of Echinacea extract as claimed in claim 1 is characterized in that comprising the following step:
(1) extraction, concentrated and centrifugal: the Echinacea medical material is extracted with ethanol water, extracting solution is concentrated, centrifugal then, get supernatant;
(2) membrance separation: with the supernatant thin up of step (1) gained, dilute liquid medicine filters through organic membrane, ultrafilter membrane and NF membrane successively, and filtrate is Echinacea extract.
3. preparation method as claimed in claim 2 is characterized in that:
In the step (1), described Echinacea medical material is the medical material after pulverizing; The temperature of described extraction is 70 ℃～100 ℃; The concentration of described ethanol water is percent by volume 10%～60%; The each consumption that extracts of described ethanol water is 8～12 times of Echinacea medical material weight; The number of times of described extraction is 1～3 time, and each time is 0.5～2 hour; Described simmer down to is with 1/3 of extracting solution simmer down to original liquid volume; Described centrifugal rotation speed is 4000～5000r/min.
4. preparation method as claimed in claim 3 is characterized in that: the particle diameter of described Echinacea medical material is 40 orders; The temperature of described extraction is a reflux temperature.
5. preparation method as claimed in claim 2 is characterized in that:
In the step (2), described water is deionized water; The consumption of described water is 2 times of supernatant volume; The pore size filter of described organic membrane is 250～400nm, and the material of organic membrane is the hydrophilic polyvinylidene fluoride; The pore size filter of described ultrafilter membrane is 5～15nm, and the material of ultrafilter membrane is the hydrophilic polyvinylidene fluoride; The pore size filter of described NF membrane is 0.1～1nm, and the material of NF membrane is a polyamide; It is 0～0.5Mpa that described process organic membrane carries out filtering operating pressure; It is 0～0.8Mpa that described process ultrafilter membrane carries out filtering operating pressure; It is 0～3Mpa that described process NF membrane is carried out filtering operating pressure; Operative temperature when above-mentioned three kinds of films filter is 20 ℃～35 ℃.
6. preparation method of extract as claimed in claim 5 is characterized in that: it is 0.2Mpa that described process organic membrane carries out filtering operating pressure; It is 0.6Mpa that described process ultrafilter membrane carries out filtering operating pressure; It is 1.5Mpa that described process NF membrane is carried out filtering operating pressure.
7. preparation method of extract as claimed in claim 2 is characterized in that: in the step (2), also comprise the steps: to collect the NF membrane filtrate filtered after described filtration, this filtrate is carried out drying, obtain the Echinacea extract powder.
8. preparation method as claimed in claim 2 is characterized in that: described preparation method comprises the following step:
(a) ethanol water reflux, extract: with Echinacea pulverizing medicinal materials to 40 order, add percent by volume 40%～60% ethanol water reflux, extract, 2 times, each consumption is 8～12 times of amounts of Echinacea medical material weight, and each time is 0.5～2 hour, merges 40%～60% ethanol extract; Residue adds 10%～20% ethanol water reflux, extract,, and consumption is 8～12 times of amounts of Echinacea medical material weight, and the time is 1 hour, merges 40%～60% ethanol extract and 10%～20% ethanol extract then;
(b) concentrate: the extracting solution of step (a) gained is concentrated into 1/3 of original liquid volume;
(c) centrifugal: the medicinal liquid of step (b) gained is centrifugal with 4000～5000r/min, get supernatant;
(d) membrance separation: get supernatant, adding is that the deionized water of 2 times of supernatant volumes fully dilutes, and dilute liquid medicine is further purified through organic membrane, ultrafilter membrane and NF membrane successively, the filtrate after the collection nanofiltration; Adopt the piece-rate system of membrance separation to be: the pore size filter of organic membrane is 250～400nm, and the material of organic membrane is the hydrophilic polyvinylidene fluoride; The pore size filter of ultrafilter membrane is 5～15nm, and the material of ultrafilter membrane is the hydrophilic polyvinylidene fluoride; The pore size filter of described NF membrane is 0.1～1nm, and the material of NF membrane is a polyamide; It is 0～0.5Mpa that described organic membrane carries out filtering operating pressure; It is 0～0.8Mpa that described ultrafilter membrane carries out filtering operating pressure; It is 0～3Mpa that described NF membrane is carried out filtering operating pressure; Operative temperature when above-mentioned three kinds of films filter is 20 ℃～35 ℃;
(e) spray drying: carry out spray drying through the NF membrane filtrate filtered, obtain the Echinacea extract powder.
9. as each described preparation method of claim 2～8, it is characterized in that: described Echinacea medical material is selected from genus echinacea plant Echinacea, Echinacea angustifolia or white Echinacea.
10. the detection method of content of phenols component in the Echinacea extract is characterized in that it comprises following condition: detect with efficient liquid-phase chromatography method; With the octadecylsilane chemically bonded silica is filler; With acetonitrile and volumetric concentration is that 0.1% phosphoric acid solution is that eluent carries out gradient elution, and actual conditions sees Table 1; The detection wavelength is 330nm, and column temperature is 35 ℃, and flow velocity is 1.5ml/min;
Table 1
With caffeoyl tartaric acid, echinacoside and chicoric acid is reference substance; Above percentage ratio is percent by volume.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102531900A (en) * | 2010-12-20 | 2012-07-04 | 沈阳双鼎制药有限公司 | Caftaric acid as well as preparation method and applications thereof |
| CN102716164A (en) * | 2012-06-28 | 2012-10-10 | 齐鲁动物保健品有限公司 | Echinacea extract and preparation method of echinacea extract |
| CN107028996A (en) * | 2017-04-11 | 2017-08-11 | 山西中医学院 | A kind of detection method of Chinese Herba Ixeritis Denticulatae extract and its preparation method and its organic acid composition |
| CN110393735A (en) * | 2018-04-19 | 2019-11-01 | 李克英 | A kind of drug extract and liquid medicine |
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2008
- 2008-12-30 CN CN200810205105A patent/CN101766667A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102531900A (en) * | 2010-12-20 | 2012-07-04 | 沈阳双鼎制药有限公司 | Caftaric acid as well as preparation method and applications thereof |
| CN102716164A (en) * | 2012-06-28 | 2012-10-10 | 齐鲁动物保健品有限公司 | Echinacea extract and preparation method of echinacea extract |
| CN107028996A (en) * | 2017-04-11 | 2017-08-11 | 山西中医学院 | A kind of detection method of Chinese Herba Ixeritis Denticulatae extract and its preparation method and its organic acid composition |
| CN110393735A (en) * | 2018-04-19 | 2019-11-01 | 李克英 | A kind of drug extract and liquid medicine |
| CN110393735B (en) * | 2018-04-19 | 2021-07-20 | 李克英 | Medicinal extract and medicinal liquor |
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