CN103768151A - Application of osmanthus phenylethanoid glycoside extract in preparing anti-aging drugs or health products - Google Patents
Application of osmanthus phenylethanoid glycoside extract in preparing anti-aging drugs or health products Download PDFInfo
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Abstract
The invention discloses application of an osmanthus phenylethanoid glycoside extract in preparing anti-aging drugs or health products. The total phenylethanoid glycoside content in the osmanthus phenylethanoid glycoside extract is 30-90 wt%, and the total phenylethanoid glycosides comprise verbascoside and isoverbascoside. The verbascoside content in the osmanthus phenylethanoid glycoside extract is 25-80 wt%, and the weight ratio of the verbascoside to the isoverbascoside in the total phenylethanoid glycosides is 48:1-300:1.
Description
Technical field
The present invention relates to agricultural byproducts intensive processing and comprehensive utilization field.Relate more specifically to a kind of phenethyl alcohol glycoside extract extracting and method for making thereof and purposes-for the preparation of antiaging agent or health product from Flos Osmanthi Fragrantis.
Background technology
Flos Osmanthi Fragrantis, have another name called wooden slippers, rock osmanthus, one of China tradition ten large flowers, extensively plant in Basin of Huaihe River and areas to the south, China has formed several large Flos Osmanthi Fragrantis commoditys production base such as Zhejiang Hangzhou, Anhui six peaces, xianning,hubei, Fauna of Taoyuan, Nw Hunan, Law Firm Suzhou Jiangsu, Guilin, Wuhan, Hubei and Chengdu, Sichuan at present.Osmanthus cultivars is various, and nearly 152 kinds, can be divided into four strains, i.e. four seasons osmanthus, Osmanthus tragranscv.Aurantiacu, silver-colored osmanthus, Osmanthus fragrans var.thunbergii..Flos Osmanthi Fragrantis, except viewing and admiring and beautifying, also has higher nutrition and medical value.The traditional Chinese medical science thinks that Flos Osmanthi Fragrantis is the length of hundred medicines, with wine appetizing refreshment, the stomach invigorating tonify deficiency of Flos Osmanthi Fragrantis brew, can reach the effect of " the longevity Your Highness of drink ", and osmanthus flower tea has looks improving and the skin nourishing, the throat of releiving, improve the effects such as excessive phlegm cough.Flos Osmanthi Fragrantis is also made into the cuisines such as Oryza glutinosa Flos Osmanthi Fragrantis Rhizoma Nelumbinis, sweet-scented cake, Flos Osmanthi Fragrantis almond curd in syrup, by the general common people is liked.
But, people are also considerably less to the research of the many functional components in Flos Osmanthi Fragrantis up to now, mainly concentrate on Flos Osmanthi Fragrantis and compose fragrant composition and a few medicinal ingredient, as linalool, γ-decalactone, alpha, beta-lonone, 4-hydrogen-alpha, beta-lonone, Palmic acid, alpha-linolenic acid.Also have part to carry out the research of separation and Extraction purification to the flavones in Flos Osmanthi Fragrantis and Polyphenols component, but only limit to the research of crude extract, have no the analysis of monomeric compound.
Inventor's patent of invention 201310169455.1 in earlier stage discloses a kind of Flos Osmanthi Fragrantis polyphenol extract, the weight content of its phenolic acid is 0.5%～2%, the weight content of phenethyl alcohol glycoside is 50%～80%, the weight content of its Content of Chlorogenic Acid is 40%～70%, chlorogenic acid, caffeic acid and P-coumaric acid mass ratio are 25～50:5～15:6～10, and in phenethyl alcohol glycoside, the weight content of verbascoside is 80%～95%; This patent also discloses a kind of preparation method-high-pressure microwave extraction method simultaneously.But along with going deep into of research, we find also to contain in Flos Osmanthi Fragrantis other the phenethyl alcohol glycoside compounds except verbascoside.In addition, during traditional Flos Osmanthi Fragrantis polyphenol extracts, do not pay close attention to the stability of Phenylethanoid glycosides, therefore affect to some extent extracting yield and extract purity, therefore, need in leaching process, take measures to prevent oxidation and the decomposition of phenethyl alcohol glycoside.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract that contains different verbascoside in the application of preparing in antiaging agent or health product.
In order to solve the problems of the technologies described above, the invention provides a kind of Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract in the application of preparing in antiaging agent or health product.
As Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of the present invention in the improvement of preparing the application in antiaging agent or health product:
In Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, phenylethanoid glycosides content is 30～90%(% by weight), described phenylethanoid glycosides comprises verbascoside, different verbascoside.
As Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of the present invention in the further improvement of preparing the application in antiaging agent or health product: in described Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, verbascoside content is 25～80%(% by weight), in phenylethanoid glycosides, verbascoside is 48:1～300:1 with the ratio of the weight of different verbascoside.
Remarks explanation: verbascoside accounts for 90% left and right of phenylethanoid glycosides content.
As Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of the present invention in the further improvement of preparing the application in antiaging agent or health product: in described Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, phenylethanoid glycosides content is 40～80%;
In described Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, verbascoside content is 35～70%, and in phenylethanoid glycosides, verbascoside is that 48:1～150:1(is for example 48:1 with the ratio of the weight of different verbascoside, 77:1,80～150:1).
As Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of the present invention in the further improvement of preparing the application in antiaging agent or health product: the preparation method of Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract comprises the following steps:
(a), by broken Flos Osmanthi Fragrantis dry flower (moisture≤10%) (approximately 20～40 object powder), be added in ethanol water, then add the aqueous solution of antioxidant or antioxidant, then add weak acid until pH is 4～6, obtain extraction solution;
In described ethanol water, the volumetric concentration of ethanol is 30～99.9%(v/v); Above-mentioned concentration is preferably 50～90%;
The ethanol water of described every 1KG Flos Osmanthi Fragrantis dry flower adapted 10～15L;
The weight ratio of described antioxidant and Flos Osmanthi Fragrantis dry flower is: 0.05～10%; Above-mentioned weight ratio is preferably 0.2%;
(b), extraction solution is carried out at 50～80 ℃ to lixiviate 1.5～3.0 hours, be cooled to after room temperature, filter or centrifugal, obtain extracting solution;
(c), by extracting solution directly through concentrating under reduced pressure reclaim ethanol, obtain concentrated solution; Again by concentrated solution dilute with water, until the pH of gained diluent is 4-6;
(d), diluent is adsorbed to the ethanol water eluting that is 20～50% by volumetric concentration through adsorbent resin;
(e), after eluent concentrating under reduced pressure, dry (for example for spraying is dry, low pressure dry or microwave drying), obtains Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract.
As Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of the present invention in the further improvement of preparing the application in antiaging agent or health product:
Described antioxidant is ascorbic acid, ascorbyl palmitate, arabo-ascorbic acid, sodium erythorbate, vitamin E, carotenoid, Folium Bambusae antioxidant or tea polyphenols;
Described weak acid is formic acid, acetic acid, hydroxyacetic acid, lactic acid, tartaric acid, malic acid, fumaric acid, ascorbic acid, cinnamic acid, benzoic acid, ferulic acid, caffeic acid, gallic acid or phosphoric acid.
As Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of the present invention in the further improvement of preparing the application in antiaging agent or health product: described Flos Osmanthi Fragrantis is Osmanthus fragrans var.thunbergii., silver-colored osmanthus, four seasons osmanthus or Osmanthus tragranscv.Aurantiacu.
As Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of the present invention in the further improvement of preparing the application in antiaging agent or health product: preparation method comprises the following steps:
(a), 1kg Osmanthus tragranscv.Aurantiacu dry flower fragmentation (moisture≤10%) is crushed to and can crosses 20 object sieves, be added to 10L volumetric concentration and be in 90% ethanol water, add AOB solution 2L, utilizing 1mol/L acetic acid aqueous solution to adjust pH is 5, obtains extraction solution again;
In described every liter of AOB solution, contain 1g AOB;
(b), extraction solution is carried out at 50～80 ℃ to lixiviate 2 hours, be cooled to after room temperature, filter or centrifugal, obtain extracting solution;
(c), by extracting solution directly through concentrating under reduced pressure reclaim ethanol, obtain concentrated solution; Again by concentrated solution dilute with water, until the pH of gained diluent is 4;
(d), diluent is adsorbed to the ethanol water eluting that is 30% by volumetric concentration through adsorbent resin;
(e), after eluent concentrating under reduced pressure, spray-dried, low pressure is dried or microwave drying, can obtain Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract.
As Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of the present invention, in the application of preparing in antiaging agent or health product, preparation method comprises the following steps:
(a), 1kg Osmanthus fragrans var.thunbergii. dry flower fragmentation (moisture content≤10%) is crushed to and can crosses 20 object sieves, being added to 15L volumetric concentration is in 80% ethanol water, add arabo-ascorbic acid sodium water solution 2L, utilizing the adjustment of 1mol/L aqueous formic acid to extract pH value of solution is 5, obtains extraction solution again;
In every liter of arabo-ascorbic acid sodium water solution, contain 1g sodium erythorbate;
(b), extraction solution is carried out at 50～80 ℃ to lixiviate 2 hours, be cooled to after room temperature, filter or centrifugal, obtain extracting solution;
(c), extracting solution is reclaimed to ethanol through concentrating under reduced pressure, obtain concentrated solution; Dilute with water again, until the pH of gained diluent is 5;
(d), diluent is adsorbed to the ethanol water eluting that is 30% by volumetric concentration through adsorbent resin;
(e), after eluent concentrating under reduced pressure, spray-dried, low pressure is dried or microwave drying, obtains Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract.
In the present invention, room temperature generally refers to 10～25 ℃.
The inventor, through further investigation for many years, has carried out extracting separation to the various compositions of Flos Osmanthi Fragrantis, has obtained Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, and the research of this extract is shown, this extract is mainly containing compositions such as verbascoside, different verbascosides.Complete on this basis the present invention.
As used herein, Flos Osmanthi Fragrantis (Osmanthus fragrans) refers to the flower of osmanthus fragrans.
The raw material that the present invention adopts can carry out pretreatment, also can be without pretreatment.A kind of preferred feedstock is the Flos Osmanthi Fragrantis of powder type.For example, collect fresh Flos Osmanthi Fragrantis, pulping squeezing or collection Flos Osmanthi Fragrantis dry flower, be crushed to approximately 20～40 object powder.
Can be used for osmanthus cultivars of the present invention and be not particularly limited, can be the Flos Osmanthi Fragrantis of different cultivars, preferably Osmanthus fragrans var.thunbergii., silver-colored osmanthus, four seasons osmanthus, Osmanthus tragranscv.Aurantiacu.
Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of the present invention is a kind of take verbascoside, different verbascoside as main mixture.With spectrophotometry, take verbascoside as standard substance, the content that records phenylethanoid glycosides in extract is 30～90% (being preferably 40～80%); Use HPLC technical Analysis, in extract, verbascoside content is 25～80% (being preferably 35～70%), and verbascoside is 48:1～300:1 (being preferably 48:1～150:1) with the ratio of different verbascoside content.
Take pharmaceutical composition or Halth-care composition as example, they can be solid-state (as granule, tablet, lyophilized powder, suppository, capsule, sublingual lozenge) or liquid (as oral liquid) or other suitable shapes.The content of Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of the present invention is generally 1%～99% of composition weight, is preferably 2%～96%, is more preferably 5%～90%, and best 15%～80%.
Halth-care composition can be single dose or multi-agent form.By application dosage, conventionally contain 10～2000mg/ agent, preferably approximately 20～1000mg/ agent, more preferably 50～500mg/ agent.
Pharmaceutical composition of the present invention or Halth-care composition can carry out administration by conventional route, and optimal way is oral.Pharmaceutical preparation should match with administering mode.Amount of application of the present invention, calculates by active substance, is generally Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract 0.1～500mg/kg body weight every day, preferably about 0.5～50mg/kg body weight.In addition, preparation of the present invention also can use together with other auxiliary agents, and for example, other auxiliary agents comprise various existing anti-cancer active matters or anti-oxidation active substance.
Major advantage of the present invention is:
(a) provide a kind of originate wide, form distinct, best in quality, quality controllable, of many uses and there is the Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of defying age purposes.
(b) realized the high efficiency extraction of phenethanol glucosides in Flos Osmanthi Fragrantis by the technology of the present invention, and technological operation is easy, the Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract quality obtaining is good, stay in grade.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Fig. 1 is the liquid chromatogram of Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract.
Fig. 2 is the liquid chromatogram of verbascoside and different verbascoside.
Fig. 3 is the chemical structural drawing of verbascoside and different verbascoside.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.The experimental technique of unreceipted actual conditions in the following example, conventionally according to normal condition, or the condition of advising according to manufacturer.
Universal method
1) phenylethanoid glycosides assay:
50.0mg Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract is dissolved in to methanol, be settled to 100ml, get 3ml and add use ultraviolet spectrophotometer in quartz colorimetric utensil to detect its light absorption value, replication 3 times at 338nm place, take verbascoside as standard substance, calculate phenylethanoid glycosides content according to standard curve.
2) verbascoside and different verbascoside assay-high performance liquid chromatography (HPLC) in Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract:
Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract adds 2%(volume %) acetic acid solution dissolving, make 500 μ g/mL solution, cross 0.45 μ m film, sample introduction.High performance liquid chromatograph device: Shimadzu LC-2010A high performance liquid chromatogram, SPD-20A UV-detector, BDS C18 post (4.6mm × 250mm, 5 μ m i.d.), mobile phase: acetonitrile: 2% acetum (volume ratio of 20:80), detects wavelength: 330nm, flow velocity: 0.8mL/min, column temperature: 35 ℃, sampling volume 10 μ L.Take verbascoside and different verbascoside as standard substance, qualitative according to retention time, quantitative according to peak area external standard method.
Embodiment 1:
By 1kg Osmanthus fragrans var.thunbergii. dry flower fragmentation (moisture content≤10%, be crushed to and can cross 20 object sieves), add the 80%(volume % of 15L) in ethanol water, add again 0.1% arabo-ascorbic acid sodium water solution (, in described every liter of arabo-ascorbic acid sodium water solution, contain 1g sodium erythorbate) 2L, utilizes the adjustment of 1mol/L aqueous formic acid to extract pH value of solution in 5 left and right; At temperature 50 C～80 ℃, carry out lixiviate 2 hours, be cooled to after room temperature, filter and obtain extracting solution; Extracting solution, directly through concentrating under reduced pressure (in 0.010～0.100MPa, temperature is 50～60 ℃), is reclaimed to ethanol, obtain concentrated solution (about 4L), then dilute with water, until diluent pH is 5 left and right; By diluent through adsorbent resin absorption (adsorbent resin is HPD300, and consumption is 1L), with 30%(volume %) ethanol water 2L eluting; After eluent concentrating under reduced pressure (in 0.010～0.100MPa MPa, temperature is 75～90 ℃), spray-dried (inlet temperature is 180～200 ℃, and leaving air temp is 85～95 ℃), can obtain Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract powder 184g.
Extract is carried out to component analysis, result is: in Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, phenylethanoid glycosides content is 75.3%, Fig. 1-3 show, Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract contains verbascoside (69.4%) and different verbascoside (0.9%), verbascoside: different verbascoside=77:1(weight ratio).
Comparative example 1-1, " the 80%(volume % of 15L) ethanol water " in embodiment 1 made into " straight alcohol of 12L ", all the other are with embodiment 1.
Finally can obtain Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract powder 171g.In the Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of gained, phenylethanoid glycosides content is 70.5%, and Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract contains verbascoside (65.6%) and different verbascoside (0.9%).
Comparative example 1-2, " the 80%(volume % of 15L) ethanol water " in embodiment 1 made into " the 60%(volume % of 20L) ethanol water ", all the other are with embodiment 1.
Finally can obtain Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract powder 187g.In the Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of gained, phenethyl alcohol glycoside content is 71.2%, and Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract contains verbascoside (67.3%) and different verbascoside (0.8%).
Comparative example 2-1, " 0.1% arabo-ascorbic acid sodium water solution 2L " made into: 0.04% arabo-ascorbic acid sodium water solution (, containing 0.4g sodium erythorbate in described every liter of arabo-ascorbic acid sodium water solution) 2L; All the other are with embodiment 1.
Finally can obtain Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract powder 123.8g.In the Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of gained, phenylethanoid glycosides content is 25.2%, and Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract contains verbascoside (23.4%) and different verbascoside (0.2%).
Comparative example 2-2, general " 0.1%(quality %) arabo-ascorbic acid sodium water solution 2L " make into: 1.0% arabo-ascorbic acid sodium water solution (, containing 10g sodium erythorbate in described every liter of arabo-ascorbic acid sodium water solution) 2L; All the other are with embodiment 1.
Finally can obtain Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract powder 172.7g.In the Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of gained, phenylethanoid glycosides content is 75.3%, and Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract contains verbascoside (69.4%) and different verbascoside (0.9%).
Comparative example 3-1 regulates 3.5 by adjusting pH to 5 instead, and all the other are with embodiment 1.
Finally can obtain Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract powder 160.6g.In the Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of gained, phenylethanoid glycosides content is 64.2%, and Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract contains verbascoside (60.5%) and different verbascoside (0.7%).
Comparative example 3-2 regulates 6.5 by adjusting pH to 5 instead, and all the other are with embodiment 1.
Finally can obtain Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract powder 151.9g.In the Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of gained, phenylethanoid glycosides content is 61.1%, and Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract contains verbascoside (56.8%) and different verbascoside (0.7%).
Comparative example 4-1, " at 50 ℃～80 ℃, carrying out lixiviate 2 hours " made into " at 30 ℃～49 ℃, carrying out lixiviate 4 hours ", all the other are with embodiment 1.
Finally can obtain Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract powder 142.8g.In the Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of gained, phenylethanoid glycosides content is 74%, and Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract contains verbascoside (68.5%) and different verbascoside (0.85%).
Comparative example 4-2, " at 50 ℃～80 ℃, carrying out lixiviate 2 hours " made into " at 90 ℃～100 ℃, carrying out lixiviate 2 hours ", all the other are with embodiment 1.
Finally can obtain Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract powder 194.6g.In the Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of gained, phenylethanoid glycosides content is 70.5%, and Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract contains verbascoside (66.8%) and different verbascoside (0.9%).
Embodiment 2:
By 1kg four seasons osmanthus dry flower fragmentation (moisture content≤10%, be crushed to and can cross 20 object sieves), add the 90%(volume % of 10L) in ethanol water, add again 0.2% aqueous ascorbic acid (, in described every liter of aqueous ascorbic acid, contain 2g ascorbic acid) 2L, utilizes the adjustment of 0.5mol/L acetic acid aqueous solution to extract pH value of solution in 4 left and right; At temperature 50 C～80 ℃, carry out lixiviate 2 hours, be cooled to after room temperature, filter and obtain extracting solution; Extracting solution, directly through concentrating under reduced pressure (in 0.010～0.100MPa, temperature is 50～60 ℃), is reclaimed to ethanol, obtain concentrated solution (about 1.5L), then dilute with water, until diluent pH is 4 left and right; By diluent through adsorbent resin absorption (described adsorbent resin is HPD300, and consumption is 1L), with 30%(volume %) ethanol water 2L eluting; After eluent concentrating under reduced pressure (in 0.010～0.100MPa MPa, temperature is 75～90 ℃), through microwave drying (technological parameter is: microwave power 500W, microwave irradiation time 60min), can obtain Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract powder 234g.
Extract is carried out to component analysis, in result Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, phenylethanoid glycosides content is 47.3%, Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract contains verbascoside (40.5%) and different verbascoside (0.2%), verbascoside: different verbascoside=203(weight ratio).
Embodiment 3:
By 1kg Osmanthus tragranscv.Aurantiacu dry flower fragmentation (moisture content≤10%, be crushed to and can cross 20 object sieves), be added to the 90%(volume % of 10L) in alcoholic solution, add again 0.1% AOB aqueous solution (, in described every liter of AOB aqueous solution, contain 1g AOB) 2L, utilizes the adjustment of 1mol/L acetic acid aqueous solution to extract pH value of solution in 5 left and right; Must extract solution; Extraction solution is carried out to lixiviate 2 hours at temperature 50 C～80 ℃, be cooled to after room temperature, filter and obtain extracting solution; Extracting solution, directly through concentrating under reduced pressure (in 0.010～0.100MPa, temperature is 50～60 ℃), is reclaimed to ethanol, obtain concentrated solution (about 2.5L), then dilute with water, until diluent pH is 4 left and right; By diluent through adsorbent resin absorption (described adsorbent resin is HPD300, and consumption is 1L), with 30%(volume %) ethanol water 2L eluting; After eluent concentrating under reduced pressure (in 0.010～0.100MPa MPa, temperature is 75～90 ℃), through microwave drying (technological parameter is: microwave power 500W, microwave irradiation time 60min), can obtain Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract powder 258g.
Extract is carried out to component analysis, in result Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, phenylethanoid glycosides content is 74.5%, Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract contains verbascoside (68.9%) and different verbascoside (1.4%), verbascoside: different verbascoside=48(weight ratio).
Embodiment 4:
By 1kg silver osmanthus dry flower fragmentation (moisture content≤10%, be crushed to and can cross 20 object sieves), add the 50%(volume % of 15L) in alcoholic solution, add again 0.1% aqueous ascorbic acid (, in described every liter of aqueous ascorbic acid, contain 1g ascorbic acid) 2L, utilize the adjustment of 1mol/L acetic acid aqueous solution to extract pH value of solution in 4 left and right, obtain extraction solution; Extraction solution is carried out to lixiviate 2 hours at temperature 50 C～80 ℃, be cooled to after room temperature, filter, obtain extracting solution; Extracting solution, directly through concentrating under reduced pressure (in 0.010～0.100MPa, temperature is 50～60 ℃), is reclaimed to ethanol, obtain concentrated solution (about 10L), then dilute with water, until diluent pH is 4 left and right; By diluent through adsorbent resin absorption (described adsorbent resin is HPD300, and consumption is 1L), with 30%(volume %) ethanol water 2L eluting; After eluent concentrating under reduced pressure (in 0.010～0.100MPa MPa, temperature is 75～90 ℃), through microwave drying (technological parameter is: microwave power 500W, microwave irradiation time 60min), can obtain Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract powder 107g.
Extract is carried out to component analysis, in result Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, phenylethanoid glycosides content is 86.1%, Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract contains verbascoside (79.3%) and different verbascoside (0.3%), verbascoside: different verbascoside=264(weight ratio).
Embodiment 5, removing free radical
(1) DPPH method
The DPPH that accurately takes 20mg before experiment is dissolved in appropriate methanol, is settled to 500ml.Take 25-800 μ M Trolox as reference substance, get sample or the reference substance solution 100ul of dilution certain multiple, add 3.9mlDPPH, 37 ℃ of lucifuge reaction 60min, survey absorbance in 515nm wavelength place.Take Trolox concentration as abscissa, light absorption value is that vertical coordinate is made standard curve, and according to standard curve calculation sample oxidation resistance, result represents (mmol Trolox/g DW) with Trolox equivalent in every gram of extract.
(2) ABTS method
Configure respectively 7.4mM ABTS and 2.6mM potassium peroxydisulfate, equal-volume mixes before use, and 37 ℃ of lucifuge reaction 12h, dilute 27 times and use afterwards.Take 25-800 μ M Trolox as reference substance, get sample or reference substance solution 100ul after dilution certain multiple, add 3.0ml ABTS reactant liquor, after 37 ℃ of lucifuge reaction 60min, survey absorbance in 734nm place.Take Trolox concentration as abscissa, light absorption value is that vertical coordinate is made standard curve, and according to standard curve calculation sample oxidation resistance, result represents (mmol Trolox/g DW) with Trolox equivalent in every gram of extract.
(3) FRAP method
The configuration 10mM TPTZ solution take 40mM HCl as solvent, 20mM FeCl
3aqueous solution, 300mM, pH=3.6 sodium acetate buffer, three is with 1:1:10(v/v/v) be mixed to get FRAP.With FeSO
4for reference substance, get sample or reference substance solution 100ul after dilution certain multiple, add 3.0ml FRAP reactant liquor, after 37 ℃ of lucifuge reaction 60min, survey absorbance in 595nm place.Take FeSO4 concentration as abscissa, light absorption value is that vertical coordinate is made standard curve, and according to standard curve calculation sample oxidation resistance, result represents (mmol FeSO with FeSO4 equivalent in every gram of extract
4/ g DW).
(4) ORAC method
Configuration pH7.4, concentration is 75mM phosphate buffer, preparation fluorescein and AAPH solution take it as solvent.Take 0-80 μ M Trolox as reference substance, in black enzyme mark 96 orifice plates, add 20ul sample (after dilution certain multiple), 120ul fluorescein respectively, after 37 ℃ of insulation 5min, add 60ul AAPH, make fluorescein and AAPH final concentration be respectively 70nM and 12mM, enter immediately fluorescence microplate reader and measure.Condition determination is that every 2min measures once, continues 3h, and excitation wavelength and emission wavelength are respectively 485nm, 530nm.Take Trolox concentration as abscissa, light absorption value is that vertical coordinate is made standard curve, and according to standard curve calculation sample oxidation resistance, result represents (mmol Trolox/g DW) with Trolox equivalent in every gram of extract.
Result is as shown in table 1, and the Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of embodiment 1,3,4 preparation has stronger removing free radical, antioxidative ability, and is better than embodiment 1 in patent of invention [201310169455.1] and prepares gained Flos Osmanthi Fragrantis polyphenol extract.
Table 1 Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract is removed free radical ability
Note: Flos Osmanthi Fragrantis polyphenol extract is for preparing gained according to embodiment 1 in patent of invention [201310169455.1].
Embodiment 6, anti-aging effects research
The Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract that this experiment selects the present invention to prepare, adopts corn culture medium to raise fruit bat and two kinds of methods of mice are fed in the filling of preparation variable concentrations solution, to observe the antidotal effect of Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract.
1, Drosophila melanogaster is put into and is contained 0.2%(quality %) the Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of embodiment 1,3,4 or the culture tube of Flos Osmanthi Fragrantis polyphenol extract preparation raise, and take the culture tube that do not add Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract as blank group, is divided into four groups.200 left and right of each dosage group fruit bat, male and female half and half, every group establish 4 parallel.Every day is each observation once sooner or later, and the mortality of statistics fruit bat and existence number, until all dead.Respectively organize the length in life-span, record its half death time, maximum life span and average life.
The formula of above-mentioned culture medium is: water 76g, agar 1.5g, sugared 13.5g, Semen Maydis powder 10g, yeast powder 0.7g, propanoic acid 0.5mL.Preparation method is: get the half of answering amount of water, add agar to boil and stir thawing, add white sugar; Get second half water by Semen Maydis powder furnishing pasty state, join in agar water and stir and be cooked into pasty state, add 0.5ml propanoic acid to stir, be distributed into culture bottle, approximately 2cm is high, tampon beyond the Great Wall; Autoclaving, 15 pounds/cm
2, 20 points of kinds, add the paper of perching of yeast and sterilizing after cooling.
2, select 60 healthy Kunming mouses, be divided at random 6 groups: be i.e. Normal group, model control group, Flos Osmanthi Fragrantis polyphenol extract (500mg/kg), enforcement 1, enforcement 3, enforcement 4 Flos Osmanthi Fragrantis phenethyl alcohol glycoside extracts (500mg/kg).Modeling method adopts mice aging model, with the D-galactose solution of normal saline configuration 10%, except Normal group, make mice aging model in the subcutaneous D-galactose solution of injecting respectively 0.14g/kg of nape portion all the other 4 groups of every days, gives continuously D-galactose 50 days.From second week, to the mice of administration group, every day is Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract or the Flos Osmanthi Fragrantis polyphenol extract of gavage 500mg/kg respectively; Blank group, model group control group mice gavage equivalent normal saline.Sign behavior and the active situation thereof of every day timing observed and recorded mice, record the body weight change, hair luster degree, the situation of searching for food of mice, sensitivity to irritant reaction, mobbing reaction, drowsiness degree etc.After last administration 2h, take out brain, spleen, kidney, liver, suck blood, cut off fat, mesentery.By mouse spleen, after normal saline is cleaned, remove organ surface moisture with filter paper is sticky, weigh and calculate index and spleen index.Brain, spleen, kidney, liver are prepared into 10% tissue homogenate, by test kit illustration method, measure respectively SOD and MDA content in the brain, spleen, kidney, liver of mice.Experimental data adopt SPSS20.0 statistical software carry out variance analysis, result with
represent, between group, adopt t check to add up.
Through observation, record, complete after life span of drosophila melanogaster counting, the experimental data of gained is carried out to statistical analysis, result shows, compared with not dosing group in culture medium, the Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of embodiment 1,3,4 and Flos Osmanthi Fragrantis polyphenol extract half survival time, average life and the maximum life span to fruit bat all has prolongation effect in various degree.The Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of embodiment 1,3,4 has extended 32.3%, 38.7%, 29.3% and 26.9%, 31.6%, 21.4% by the average life of female male drosophila respectively, matched group is compared, extend successful, difference has statistical significance (P<0.05), and is better than Flos Osmanthi Fragrantis polyphenol extract (13.9% and 13.3%) and the results are shown in Table 2.
The impact of table 2 Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract on life span of drosophila melanogaster
Note: compared with matched group, * P<0.05, * * P<0.01; Flos Osmanthi Fragrantis extract is for preparing gained according to embodiment 1 in patent of invention [201310169455.1].
The normal group mice mental status is good, physical agility, hair luster, be difficult for capturing; Model group mice lassitude, be slow in action, hair color is withered does not revolt while doing not gloss, depilation, crawl, be easy to capture; The above-mentioned performance of administration group mice has optimum reverse compared with model group; Embodiment 1,3,4 Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract doses group compared with normal group mice profiles are unchanged, movable as usual.D-galactose model group mouse spleen index obviously declines, and has significant difference (P<0.05) compared with Normal group, illustrates that the mouse aging immunity of D-galactose model induction obviously declines.After embodiment 1,3, the 4 Flos Osmanthi Fragrantis phenethyl alcohol glycoside extracts of gavage 500mg/kg, compared with model group, index and spleen index obviously increases, and has significant difference (P<0.05), and is better than same dosage Flos Osmanthi Fragrantis polyphenol extract, the results are shown in Table.The SOD content of normal mouse tissue is higher, and the SOD content of mouse aging tissue is lower.Embodiment 1,3,4 Flos Osmanthi Fragrantis phenethyl alcohol glycoside extracts can improve mouse brain, kidney, hepatic tissue SOD content, compared with model group, there is significant statistical significance (P<0.05 or P<0.01), be better than same dosage Flos Osmanthi Fragrantis polyphenol extract, the results are shown in Table.The MDA content of normal mouse tissue is lower, and the MDA content of mouse aging tissue is higher.Embodiment 1,3,4 Flos Osmanthi Fragrantis phenethyl alcohol glycoside extracts can reduce mouse brain, kidney, Liver MDA, compared with model group, there is significant statistical significance (P<0.05 or P<0.01), be better than same dosage Flos Osmanthi Fragrantis polyphenol extract, the results are shown in following table.
Table 3 mouse spleen index
Note: compared with model group, * P<0.05, * * P<0.01; Flos Osmanthi Fragrantis polyphenol extract is for preparing gained according to embodiment 1 in patent of invention [201310169455.1].
The impact of the sweet extract of table 4 Flos Osmanthi Fragrantis phenethanol on D-gal Aging model SOD content
Note: compared with model group, * P<0.05, * * P<0.01; Flos Osmanthi Fragrantis polyphenol extract is for preparing gained according to embodiment 1 in patent of invention [201310169455.1].
The impact of the sweet extract of table 5 Flos Osmanthi Fragrantis phenethanol on D-gal Aging model M DA content
Note: compared with model group, * P<0.05, * * P<0.01; Flos Osmanthi Fragrantis polyphenol extract is for preparing gained according to embodiment 1 in patent of invention [201310169455.1].
This experiment is first tested by drosophila survival, tentatively shows that Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract has certain anti-aging effects, and further inquires into its anti-aging effects to D-gal Aging mouse model.In experiment, adopt the classical way of injection of d-galactose to make aging model, long-term injection of d-galactose can cause general metabolism disorder, immune organ degeneration, free radical surplus etc.Experimental result shows, there is obvious old and feeble sign behavior in model mice, such as lassitude, be slow in action, the withered original text of hair color not gloss, be easy to capture etc., there is atrophy in spleen, in brain, kidney, liver, SOD content declines, MDA increased content, shows that it is successful making aging model through the injection of D-galactose.Existing known caused by free radical aging, not only threaten people's life-span, also follow the disease relevant with aging, such as senile dementia, cancer, cardiovascular and cerebrovascular disease etc., even patient's rejuvenation day by day, this becomes the formidable enemy of human health and the heavy burden of social prosperity gradually.Under normal circumstances, the generation of machine interior free yl keeps balance with elimination, but with advancing age or the impact of disease, in body, the activity of antioxidase weakens gradually, can not remove free radical in time and cause the excessive generation of lipid peroxide, make membrane structure and the function generation obstacle of cell, cause the old and feeble and dead of cell.SOD is the important antioxidase of removing free radical in body, the high mental retardation direct reaction of its content goes out the ability of body removing free radical, and MDA is the catabolite of lipid peroxide, be proportionate with age growth, the order of severity that the high mental retardation indirect reaction of its content body cell is attacked by free radical.This experimentation shows, in D-gal Aging model mice body, has produced oxidative damage, and the body accumulation amount of lipid peroxide increases.Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract can have facilitation to the activity of SOD in aging model Mice Body, and can suppress MDA content simultaneously increases, and illustrates that aging resistance effect is relevant with the activity of its raising antioxidase and the generation of inhibition lipid peroxide etc.Experimental data shows, Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract improves mouse aging hepatic tissue SOD content, it is the most obvious to reduce the effect of MDA content, illustrates that Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract protects hepatocellular effect the most obvious.Lipid peroxide major part is produced by hepatocyte, and it decomposes also mainly at liver, and MDA is the main degradation products of lipid peroxide.This experiment also shows that Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract can improve the spleen index of mouse aging, can obviously suppress the mice atrophy that spleen occurs in aging course, has the effect of protection immune organ, enhancing immunity.This shows, Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract can improve body immunity, removes oxygen-derived free radicals in body, suppresses lipid peroxidation, can defying age, the disease relevant with free radical had to preventive and therapeutic effect.
Embodiment 7, D-galactose is caused to the impact of subacute aging ability of learning and memory in mice
This experiment is based on the improvement of ability of learning and memory and is studied the antidotal effect of Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract.Select 72 of Kunming mouses, 18～22 grams of body weight, male and female half and half, before grouping, all mices are carried out to Morris water maze orientation navigation experiment one time, the time (incubation period) and the body weight that find platform according to mice, be divided into six groups by 72 mices: blank group, aging model group, embodiment 1, embodiment 3, embodiment 4 Flos Osmanthi Fragrantis phenethyl alcohol glycoside extracts, Flos Osmanthi Fragrantis polyphenol extract, 12 every group.Model group and administration group mouse carotid back subcutaneous injection 10%D-galactose 0.l mL/10gd (normal saline preparation), continuous 51 days, matched group injection equivalent normal saline; Experiment second week, embodiment 1,3, the 4 Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract solution 0.125mL/10gd (normal saline preparation) of administration group mice timing every day gavage 8% concentration, continuous 44 days, matched group and model group mouse stomach equivalent normal saline.
Morris water maze: (1) orientation navigation experiment.Morris water maze is mainly made up of round pool, removable cylindrical transparent organic glass platform, automatic production record.Round pool diameter 80cm, is highly 50cm, 25 ± 2 ℃ of water temperatures, and pond is divided into four quadrants.Platform diameter 5cm, height 18cm, is placed in third quadrant, and is positioned at the center of circle and pool wall line center, and in experimentation, position remains unchanged, lcm in underwater.Test the 45th day, after injected in mice, gavage, train, the upper and lower noon respectively once, is lasted 5 days.Mice, towards pool wall, is fixed into water spot from first quartile and puts into gently water, record its time of finding platform in 120s (incubation period), find platform relief mice on platform, to stop 20s.If mice fails to find platform in 120s, caused platform, be allowed to condition at simultaneously and on platform, stop 20s, then put back in cage, be designated as 120s incubation period.Test first four days for training period, be not counted in statistical analysis.Test the 5th day, above, afternoon, twice preclinical arithmetic equal value was as school grade.(2) space exploration experiment.Orientation navigation experiment finishes latter 24 hours, shifts out platform, is still fixed into water spot with first quartile mice is put into water gently towards pool wall, the time of measuring the number of times of mice spanning platform relevant position in 120s and stopping at platform place quadrant.
Diving tower experiment: mice diving tower instrument is the passive avoidance trained reflex case that 32cm*22.5cm*33cm is transparent, is divided into six with opaque black plastic plate, at the bottom of case, is made up of the thin copper grid of several spacing 0.5cm.The left rear corner of every has been placed a high 4.5cm, the cylindrical valve rubber of diameter 4.5cm.When experiment, mice, in reaction chamber, is adapted to 3min, then logical 24V alternating current immediately, mice is shocked by electricity, its normal reaction be rebound valve rubber to hide electric shock, energising 5min.First day is diving tower training, records mice and skip to from platform the number of times (errors number) of copper grid in 5min, as mice school grade.After 24h, cyclical test, records the errors number in time (incubation period) and the 5min that mice jumps off platform for the first time, as Memory result.If mice does not jump off platform in 5min, be designated as 300s incubation period, errors number is designated as 0 time.This experiment is carried out after space search experiment finishes.There are 2 mice behaviors too slow because aging model group has 3 mices, low dose group, are unfavorable for carrying out behavioristics's test, therefore these 5 mices do not take one's test in experiment.
Mean ± standard deviation for the data obtained (X ± S) represents, carries out one factor analysis of variance with SPSS17.0 statistical software.
Experimental result shows: respectively organize that incubation period, there is some difference, D-galactose Aging mice orientation navigation ability reduces, to mouse aging, the ability of learning and memory in orientation navigation experiment has certain improvement effect to embodiment 1,3,4 Flos Osmanthi Fragrantis phenethyl alcohol glycoside extracts, all there were significant differences compared with model group (P<0.01 or P<0.05), and the Flos Osmanthi Fragrantis polyphenol extract that is better than same dosage, the results are shown in following table.
The impact of the sweet extract of table 6 Flos Osmanthi Fragrantis phenethanol on the little genus orientation navigation experiment of subacute aging
Note: compared with model group, * P<0.05, * * P<0.01; Flos Osmanthi Fragrantis polyphenol extract is for preparing gained according to embodiment 1 in patent of invention [201310169455.1].
Experimental result shows: for subacute aging mice, the memory ability in the space search time has certain improvement effect to Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract.Embodiment 1,3,4 Flos Osmanthi Fragrantis phenethyl alcohol glycoside extracts can significantly improve subacute aging mice and pass through the number of times of original platform, improve and stop the original platform quadrant time, compared with model group, all there were significant differences (P<0.01 or P<0.05), and the Flos Osmanthi Fragrantis polyphenol extract that is better than same dosage, the results are shown in following table.
The impact of table 7 Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract on subacute aging mice space exploration experiment
Note: compared with model group, * P<0.05, * * P<0.01; Flos Osmanthi Fragrantis polyphenol extract is for preparing gained according to embodiment 1 in patent of invention [201310169455.1].
Experimental result shows: Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract has certain improvement effect to the ability of learning and memory of D-galactose Aging mice.The test of first day errors number has represented the learning capacity of mice, model group there are differences compared with blank group, there is statistical significance (P<0.05), embodiment 1,3,4 Flos Osmanthi Fragrantis phenethyl alcohol glycoside extracts can significantly reduce first day errors number, compared with model group, all there were significant differences (P>0.05), and be better than the Flos Osmanthi Fragrantis polyphenol extract of same dosage.Second day errors number and represented the memory ability of mice second day incubation period, there is significant difference (P<0.01) in model group compared with blank group, embodiment 1,3,4 Flos Osmanthi Fragrantis phenethyl alcohol glycoside extracts can significantly reduce by second day errors number, increase by second day incubation period, compared with model group, all there were significant differences (P>0.05), and be better than the Flos Osmanthi Fragrantis polyphenol extract of same dosage, the results are shown in following table 8.
The impact of the sweet extract of table 8 Flos Osmanthi Fragrantis phenethanol on the experiment of subacute aging mice diving tower
Note: compared with model group, * P<0.05, * * P<0.01; Flos Osmanthi Fragrantis polyphenol extract is for preparing gained according to embodiment 1 in patent of invention [201310169455.1].
This experiment adopts the method for the subcutaneous injection D-of nape portion galactose to build subacute aging mouse model, is tested and is found that the ability of learning and memory of model group mice obviously declines by behavioristics.Simultaneously, experimental result shows: administration group gives after different Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract solutions in gavage, in Morris water maze laboratory, shorten to some extent the incubation period of finding platform, increase and crossed over the number of times of platform and in the original platform quadrant time of staying; In the experiment of mice diving tower, first day, second day errors number reduce to some extent, and extend second day incubation period to some extent.Experimental result demonstrates administration group has the raising without degree in identification learning ability and dependent response ability.Experiment prompting: Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract has the certain D-of improvement galactose and cause the effect of subacute aging model ability of learning and memory in mice.In sum, the present invention tests by drosophila survival, proves that Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract has certain anti-aging effects, and the ability of learning and memory of D-galactose Aging mice is had to certain improvement effect, and drug effect is clear and definite, provides a kind of new selection for clinical.
Finally, it is also to be noted that, what more than enumerate is only several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, can also have many distortion.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention, all should think protection scope of the present invention.
Claims (9)
1. Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract is in the application of preparing in antiaging agent or health product.
2. Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract according to claim 1, in the application of preparing in antiaging agent or health product, is characterized in that:
In Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, phenylethanoid glycosides content is 30～90%(% by weight), described phenylethanoid glycosides comprises verbascoside, different verbascoside.
3. Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract according to claim 2 is in the application of preparing in antiaging agent or health product, it is characterized in that: in described Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, verbascoside content is 25～80%(% by weight), in phenylethanoid glycosides, verbascoside is 48:1～300:1 with the ratio of the weight of different verbascoside.
4. Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract according to claim 3, in the application of preparing in antiaging agent or health product, is characterized in that: in described Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, phenylethanoid glycosides content is 40～80%;
In described Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, verbascoside content is 35～70%, and in phenylethanoid glycosides, verbascoside is 48:1～150:1 with the ratio of the weight of different verbascoside.
According to the arbitrary described Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of claim 1～4 in the application of preparing in antiaging agent or health product, it is characterized in that:
The preparation method of Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract comprises the following steps:
(a), by Flos Osmanthi Fragrantis dry flower (moisture≤10%) fragmentation, be added in ethanol water, then add the aqueous solution of antioxidant or antioxidant, then add weak acid until pH is 4～6, obtain extraction solution;
In described ethanol water, the volumetric concentration of ethanol is 30～99.9%;
The ethanol water of described every 1KG Flos Osmanthi Fragrantis dry flower adapted 10～15L;
The weight ratio of described antioxidant and Flos Osmanthi Fragrantis dry flower is: 0.05～10%;
(b), extraction solution is carried out at 50～80 ℃ to lixiviate 1.5～3.0 hours, be cooled to after room temperature, filter or centrifugal, obtain extracting solution;
(c), extracting solution is reclaimed to ethanol through concentrating under reduced pressure, obtain concentrated solution; Dilute with water again, until the pH of gained diluent is 4～6;
(d), diluent is adsorbed to the ethanol water eluting that is 20～50% by volumetric concentration through adsorbent resin;
(e), after eluent concentrating under reduced pressure, dry, can obtain Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract.
6. Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract according to claim 5, in the application of preparing in antiaging agent or health product, is characterized in that:
Described antioxidant is ascorbic acid, ascorbyl palmitate, arabo-ascorbic acid, sodium erythorbate, vitamin E, carotenoid, Folium Bambusae antioxidant or tea polyphenols;
Described weak acid is formic acid, acetic acid, hydroxyacetic acid, lactic acid, tartaric acid, malic acid, fumaric acid, ascorbic acid, cinnamic acid, benzoic acid, ferulic acid, caffeic acid, gallic acid or phosphoric acid.
7. Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract according to claim 6, in the application of preparing in antiaging agent or health product, is characterized in that: described Flos Osmanthi Fragrantis is Osmanthus fragrans var.thunbergii., silver-colored osmanthus, four seasons osmanthus or Osmanthus tragranscv.Aurantiacu.
8. Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract according to claim 7, in the application of preparing in antiaging agent or health product, is characterized in that preparation method comprises the following steps:
(a), 1kg Osmanthus tragranscv.Aurantiacu dry flower (moisture≤10%) is crushed to and can crosses 20 object sieves, be added to 10L volumetric concentration and be in 90% ethanol water, add AOB solution 2L, utilizing 1mol/L acetic acid aqueous solution to adjust pH is 5, obtains extraction solution again;
In every liter of AOB solution, contain 1g AOB;
(b), extraction solution is carried out at 50～80 ℃ to lixiviate 2 hours, be cooled to after room temperature, filter or centrifugal, obtain extracting solution;
(c), extracting solution is reclaimed to ethanol through concentrating under reduced pressure, obtain concentrated solution; Dilute with water again, until the pH of gained diluent is 4;
(d), diluent is adsorbed to the ethanol water eluting that is 30% by volumetric concentration through adsorbent resin;
(e), after eluent concentrating under reduced pressure, spray-dried, low pressure is dried or microwave drying, obtains Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract.
9. Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract according to claim 7, in the application of preparing in antiaging agent or health product, is characterized in that preparation method comprises the following steps:
(a), 1kg Osmanthus fragrans var.thunbergii. dry flower fragmentation (moisture content≤10%) is crushed to and can crosses 20 object sieves, being added to 15L volumetric concentration is in 80% ethanol water, add arabo-ascorbic acid sodium water solution 2L, utilizing the adjustment of 1mol/L aqueous formic acid to extract pH value of solution is 5, obtains extraction solution again;
In every liter of arabo-ascorbic acid sodium water solution, contain 1g sodium erythorbate;
(b), extraction solution is carried out at 50～80 ℃ to lixiviate 2 hours, be cooled to after room temperature, filter or centrifugal, obtain extracting solution;
(c), extracting solution is reclaimed to ethanol through concentrating under reduced pressure, obtain concentrated solution; Dilute with water again, until the pH of gained diluent is 5;
(d), diluent is adsorbed to the ethanol water eluting that is 30% by volumetric concentration through adsorbent resin;
(e), after eluent concentrating under reduced pressure, spray-dried, low pressure is dried or microwave drying, obtains Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract.
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| CN107094969A (en) * | 2017-03-25 | 2017-08-29 | 浙江大学 | Sweet osmanthus soft sweets rich in acteoside and rhodioside and preparation method thereof |
| CN107722085A (en) * | 2017-10-19 | 2018-02-23 | 湖北科技学院 | The Phenylethanoid glycosides extracted from sweet osmanthus and its application and extracting method |
| CN109464450A (en) * | 2019-01-08 | 2019-03-15 | 佳木斯大学附属第医院 | A kind of drug and preparation method thereof preventing and treating cerebral apoplexy |
| CN109464450B (en) * | 2019-01-08 | 2020-03-31 | 佳木斯大学附属第一医院 | Medicine for preventing and treating cerebral apoplexy and preparation method thereof |
| CN114126578A (en) * | 2019-07-25 | 2022-03-01 | 三好化成株式会社 | Hydrophilized organic powder and cosmetic containing the same |
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