CN103768152B - Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract and its production and use - Google Patents
Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract and its production and use Download PDFInfo
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Abstract
The invention discloses a kind of Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract; In this Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, phenylethanoid glycosides content is 30 ~ 90%(% by weight), described phenylethanoid glycosides comprises verbascoside, different verbascoside.In 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.The present invention also also discloses the preparation method of above-mentioned Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract and the purposes of this Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract: for the preparation of preventing and treating the food of diabetes, medicine or health product.
Description
Technical field
The present invention relates to agricultural byproducts intensive processing and field of comprehensive utilization.Relate more specifically to a kind of phenethyl alcohol glycoside extract of extracting from Flos Osmanthi Fragrantis and method for making thereof and purposes.
Background technology
Flos Osmanthi Fragrantis, have another name called wooden slippers, rock osmanthus, one of large flowers of Chinese tradition ten, extensively plant in Basin of Huaihe River and areas to the south, current China formed Zhejiang Hangzhou, Anhui six is pacified, xianning,hubei, Fauna of Taoyuan, Nw Hunan, Law Firm Suzhou Jiangsu, Guilin, several large Flos Osmanthi Fragrantis commodity production base such as Wuhan, Hubei and Chengdu, Sichuan.Osmanthus cultivars is various, and nearly 152 kinds, can be divided into four strains, i.e. Osmanthus fragans, 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 the wine of Flos Osmanthi Fragrantis brew appetizing refreshment, stomach invigorating tonify deficiency, can reach the effect of " the longevity Your Highness of drink ", osmanthus flower tea has looks improving and the skin nourishing, 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, the research of people to the many functional components in Flos Osmanthi Fragrantis is up to now also considerably less, 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 the flavones in Flos Osmanthi Fragrantis and Polyphenols component to be carried out to the research of separation and Extraction purification, but be only limitted to the research of crude extract, have no the analysis of monomeric compound.
The present 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 in Flos Osmanthi Fragrantis also containing other the phenethyl alcohol glycoside compounds except verbascoside.In addition, traditional Flos Osmanthi Fragrantis polyphenol does not pay close attention to the stability of Phenylethanoid glycosides in extracting, and therefore extraction yield and extract purity affect to some extent, therefore, need the oxidation Sum decomposition taking measures to prevent phenethyl alcohol glycoside in leaching process.
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 containing different verbascoside and its production and use.
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 Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, phenylethanoid glycosides content is 30 ~ 90%(% by weight), described phenylethanoid glycosides comprises verbascoside, different verbascoside.
Improvement as Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of the present invention: in 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 illustrate: verbascoside accounts for about 90% of phenylethanoid glycosides content.
Operation as Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of the present invention improves: in 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 and the ratio of the weight of different verbascoside are 48:1 ~ 150:1(is such as 48:1,77:1,80 ~ 150:1).
The present invention also provides the preparation method of above-mentioned Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract simultaneously, comprises the following steps:
(a), by broken for Flos Osmanthi Fragrantis dry flower (moisture≤10%) (about 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 lixiviate 1.5 ~ 3.0 hours at 50 ~ 80 DEG C, after being cooled to 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 through adsorbent resin, be the ethanol water eluting of 20 ~ 50% by volumetric concentration;
E, after (), eluent concentrating under reduced pressure, dry (spraying dry, low pressure are dried or microwave drying), obtains Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract.
Improvement as the preparation method of Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of the present invention:
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.
Further improvement as the preparation method of Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of the present invention: Flos Osmanthi Fragrantis is Osmanthus fragrans var.thunbergii., silver-colored osmanthus, Osmanthus fragans or Osmanthus tragranscv.Aurantiacu.
As the further improvement of the preparation method of Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of the present invention, be any one method following:
Method one, to comprise the following steps:
(a), 1kg Osmanthus tragranscv.Aurantiacu dry flower (moisture≤10%) is crushed to and can crosses 20 objects sieves, being added to 10L volumetric concentration is in the ethanol water of 90%, add AOB solution 2L again, utilizing 1mol/L acetic acid aqueous solution to adjust pH is 5, obtains extraction solution;
Containing 1g AOB in often liter of AOB solution;
(b), extraction solution is carried out lixiviate 2 hours at 50 ~ 80 DEG C, after being cooled to room temperature, filter or centrifugal, obtain extracting solution;
(c), extracting solution is reclaimed 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 through adsorbent resin, be the ethanol water eluting of 30% by volumetric concentration;
E, after (), eluent concentrating under reduced pressure, spray-dried, low pressure is dried or microwave drying, obtains Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract;
Method two, to comprise the following steps:
(a), 1kg Osmanthus fragrans var.thunbergii. dry flower fragmentation (moisture content≤10%) is crushed to and can crosses 20 objects sieves, being added to 15L volumetric concentration is in 80% ethanol water, add arabo-ascorbic acid sodium water solution 2L again, utilizing the adjustment of 1mol/L aqueous formic acid to extract pH value of solution is 5, obtains extraction solution;
Containing 1g sodium erythorbate in often liter of arabo-ascorbic acid sodium water solution;
(b), extraction solution is carried out lixiviate 2 hours at 50 ~ 80 DEG C, after being cooled to room temperature, filter or centrifugal, obtain extracting solution;
(c), extracting solution is reclaimed 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 through adsorbent resin, be the ethanol water eluting of 30% by volumetric concentration;
E, after (), eluent concentrating under reduced pressure, spray-dried, low pressure is dried or microwave drying, obtains Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract.
The present invention also provides simultaneously and utilizes above-mentioned Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract to prepare and the compositions that obtains: described combination species contain the Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of 0.01 ~ 99.9wt%, and surplus is carrier.
Improvement as compositions of the present invention: compositions is pharmaceutical composition, Halth-care composition, food compositions or cosmetic composition.
The present invention also provides the purposes of above-mentioned Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract simultaneously: for the preparation of preventing and treating the food of diabetes, medicine or health product.
In the present invention, room temperature generally refers to 10 ~ 25.℃
The present inventor, through furtheing investigate for many years, has carried out extraction and isolation to the various compositions of Flos Osmanthi Fragrantis, obtains a kind of extract effectively can preventing and treating diabetes, shows the research of this extract, and this extract is mainly containing the composition such as verbascoside, different verbascoside.Complete the present invention on this basis.
As used herein, Flos Osmanthi Fragrantis (Osmanthusfragrans) refers to the flower of osmanthus fragrans.
The raw material that the present invention adopts can carry out pretreatment, also can without pretreatment.A kind of preferred feedstock is the Flos Osmanthi Fragrantis of powder type.Such as, collect fresh Flos Osmanthi Fragrantis, pulping squeezing or collection Flos Osmanthi Fragrantis dry flower, be crushed to about 20 ~ 40 object powder.
Osmanthus cultivars used in the present invention is not particularly limited, and can be the Flos Osmanthi Fragrantis of different cultivars, preferred Osmanthus fragrans var.thunbergii., silver-colored osmanthus, Osmanthus fragans, Osmanthus tragranscv.Aurantiacu.
As used herein, " active substance of the present invention " refers to Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract.Preferably, this Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract contains 30 ~ 90% phenylethanoid glycosides; In 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.
As used herein, " active substance preparation of the present invention " or " active compound of the present invention " refers to the compositions containing Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, comprises pharmaceutical composition and Halth-care composition.
Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of the present invention is a kind of based on the mixture of verbascoside, different verbascoside.With spectrophotometry, be standard substance with verbascoside, the content recording 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 in phenylethanoid glycosides, verbascoside and the ratio of different verbascoside content are 48:1 ~ 300:1 (being preferably 48:1 ~ 150:1).
Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of the present invention has the beneficial functional preventing and treating diabetes, therefore can be used for preparing relevant medicine, health product.Therefore, present invention also offers a kind of containing Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of the present invention as the compositions (comprising pharmaceutical composition, Halth-care composition and food compositions etc.) of active ingredient.These compositionss can be used for prevention, treatment or adjuvant therapy of diabetes.
After acquisition Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, it with pharmaceutically, in bromatology or on health product or cosmetics acceptable carrier, excipient or diluent mix mutually, is formed pharmaceutical composition of the present invention, food compositions or Halth-care composition by using conventional procedures.This kind of carrier comprises (but being not limited to): saline, buffer, glucose, water, glycerol, ethanol and combination thereof.
For pharmaceutical composition or Halth-care composition, 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 active component of the present invention (Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract) is generally 1 ~ 99% of composition weight, and being preferably 5 ~ 90%, is more preferably 10 ~ 85%, and best 20 ~ 80%.Pharmaceutical composition can be single dose or multi-dose formats.By applied agents gauge, usually containing 10 ~ 2000mg/ agent, preferably about 20 ~ 1000mg/ agent, more preferably 50 ~ 500mg/ agent.
Pharmaceutical composition of the present invention can carry out administration by conventional route, and optimal way is oral.Pharmaceutical preparation should match with administering mode.The amount of application of medicine of the present invention, calculates by Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, is generally about 0.1 ~ 500mg/kg body weight every day, preferably about 0.5 ~ 200mg/kg body weight.In addition, preparation of the present invention also can use together with other treatment agent.
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 prevented diabetes.
B () achieves the high efficiency extraction of phenylethanoid glycosides in Flos Osmanthi Fragrantis by the technology of the present invention, and technological operation is easy, and the Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract quality obtained 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.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.The experimental technique of unreceipted actual conditions in the following example, usually conveniently condition, or according to the condition that manufacturer advises.
Universal method
1) phenylethanoid glycosides assay:
50.0mg Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract is dissolved in methanol, be settled to 100ml, get 3ml add in quartz colorimetric utensil with ultraviolet spectrophotometer 338nm place detection its light absorption value, replication 3 times, 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 μm of film, sample introduction.The efficient liquid phase of high performance liquid chromatograph device: Shimadzu LC-2010A, SPD-20A UV-detector, BDSC18 post (4.6mm × 250mm, 5 μm of i.d.), mobile phase: acetonitrile: 2% acetum (volume ratio of 20:80), determined wavelength: 330nm, flow velocity: 0.8mL/min, column temperature: 35 DEG C, sampling volume 10 μ L.With verbascoside and different verbascoside for standard substance, qualitative according to retention time, according to peak area quantified by 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 the arabo-ascorbic acid sodium water solution of 0.1% again (namely, containing 1g sodium erythorbate in described often liter of arabo-ascorbic acid sodium water solution) 2L, utilize the adjustment of 1mol/L aqueous formic acid to extract pH value of solution about 5; At temperature 50 C ~ 80 DEG C, carry out lixiviate 2 hours, after being cooled to room temperature, filtering and obtain extracting solution; By extracting solution directly through concentrating under reduced pressure (in 0.010 ~ 0.100MPa, temperature is 50 ~ 60 DEG C), reclaim ethanol, obtain concentrated solution (about 4L), then dilute with water, until diluent pH is about 5; 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 ~ 0.100MPaMPa, temperature is 75 ~ 90 DEG C), spray-dried (inlet temperature is 180 ~ 200 DEG C, and leaving air temp is 85 ~ 95 DEG C), can obtain Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract powder 184g.
Component analysis is carried out to extract, result is: in Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, phenylethanoid glycosides content is 75.3%, Fig. 1-3 shows, 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, made into " straight alcohol of 12L " by " the 80%(volume % of 15L) ethanol water " in embodiment 1, 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 is 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 " to be made into: 0.04% arabo-ascorbic acid sodium water solution (that is, in described often liter of arabo-ascorbic acid sodium water solution containing 0.4g sodium erythorbate) 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, " 0.1%(quality %) arabo-ascorbic acid sodium water solution 2L " to be made into: 1.0% arabo-ascorbic acid sodium water solution (that is, in described often liter of arabo-ascorbic acid sodium water solution containing 10g sodium erythorbate) 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, makes adjustment pH to 5 into adjustment 3.5, 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, makes adjustment pH to 5 into adjustment 6.5, 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, " carrying out lixiviate 2 hours at 50 DEG C ~ 80 DEG C " is made into " carrying out lixiviate 4 hours at 30 DEG C ~ 49 DEG C ", 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, " carrying out lixiviate 2 hours at 50 DEG C ~ 80 DEG C " is made into " carrying out lixiviate 2 hours at 90 DEG C ~ 100 DEG C ", 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 Osmanthus fragans 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 0.2% aqueous ascorbic acid again (namely, containing 2g ascorbic acid in described often liter of aqueous ascorbic acid) 2L, utilize the adjustment of 0.5mol/L acetic acid aqueous solution to extract pH value of solution about 4; At temperature 50 C ~ 80 DEG C, carry out lixiviate 2 hours, after being cooled to room temperature, filtering and obtain extracting solution; By extracting solution directly through concentrating under reduced pressure (in 0.010 ~ 0.100MPa, temperature is 50 ~ 60 DEG C), reclaim ethanol, obtain concentrated solution (about 1.5L), then dilute with water, until diluent pH is about 4; 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 ~ 0.100MPaMPa, temperature is 75 ~ 90 DEG C), through microwave drying (technological parameter is: microwave power 500W, microwave irradiation time 60min), Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract powder 234g can be obtained.
Component analysis is carried out to extract, 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 0.1% AOB aqueous solution again (namely, containing 1g AOB in described often liter of AOB aqueous solution) 2L, utilize the adjustment of 1mol/L acetic acid aqueous solution to extract pH value of solution about 5; Solution must be extracted; Extraction solution is carried out lixiviate 2 hours at temperature 50 C ~ 80 DEG C, after being cooled to room temperature, filtering and obtain extracting solution; By extracting solution directly through concentrating under reduced pressure (in 0.010 ~ 0.100MPa, temperature is 50 ~ 60 DEG C), reclaim ethanol, obtain concentrated solution (about 2.5L), then dilute with water, until diluent pH is about 4; 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 ~ 0.100MPaMPa, temperature is 75 ~ 90 DEG C), through microwave drying (technological parameter is: microwave power 500W, microwave irradiation time 60min), Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract powder 258g can be obtained.
Component analysis is carried out to extract, 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 0.1% aqueous ascorbic acid again (namely, containing 1g ascorbic acid in described often liter of aqueous ascorbic acid) 2L, utilize the adjustment of 1mol/L acetic acid aqueous solution to extract pH value of solution about 4, obtain extraction solution; Extraction solution is carried out lixiviate 2 hours at temperature 50 C ~ 80 DEG C, after being cooled to room temperature, filtering, obtain extracting solution; By extracting solution directly through concentrating under reduced pressure (in 0.010 ~ 0.100MPa, temperature is 50 ~ 60 DEG C), reclaim ethanol, obtain concentrated solution (about 10L), then dilute with water, until diluent pH is about 4; 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 ~ 0.100MPaMPa, temperature is 75 ~ 90 DEG C), through microwave drying (technological parameter is: microwave power 500W, microwave irradiation time 60min), Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract powder 107g can be obtained.
Component analysis is carried out to extract, 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).
Active testing example
The effect of the Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract for preventing and treating diabetes of testing example 1, embodiment 3, embodiment 4 in following test case.
Embodiment 5:
Normal Wistar rats > 100, after adaptability feeds 1 week, randomly draw 8 as Normal group, common maintenance forage feed, all the other rat high glucose and high fat forage feeds, after feeding 4 weeks, fasting can't help water after 12 hours, and the modeling of lumbar injection 30mg/kg streptozotocin, after 7 days, tail vein blood surveys blood glucose, and its fasting glucose >=11.1mol/L is type 2 diabetes mellitus modeling success.Discard into mould rat, by become mould rat be divided at random model control group (gavage same volume normal saline), metformin hydrochloride group gavage 0.5g/kg, Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract embodiment 1, embodiment 3, embodiment 4 groups (low, high dose group be respectively 0.2 in phenylethanoid glycosides, 0.5g/kg), 201310169455.1 Flos Osmanthi Fragrantis polyphenol extract (in total phenols+phenethyl alcohol glycoside 0.5g/kg), verbascoside group gavage 0.5g/kg, often organize 8.Administration is after 4 weeks, and abdominal aortic blood surveys fasting glucose.Adopt SPSS20.0 software to carry out statistical analysis, compare between many groups and represent experimental result with x ± s, P < 0.05 is significant difference, and compare between group and adopt t inspection, P < 0.05 is significant difference.The result display of table 1, before medication, compared with normal group, the blood glucose value of model group rats significantly raises, and modeling success is described.Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract embodiment 1, embodiment 3, embodiment 4 groups, 201310169455.1 Flos Osmanthi Fragrantis polyphenol extract group and verbascoside group, metformin hydrochloride group each dosage group medication after 8 weeks, the blood glucose of diabetes rat all can be made obviously to reduce, and before and after medication, the blood glucose value of rat have significant difference (P < 0.05).High dose Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract significantly can reduce rat fasting blood-glucose, and reduction rate is 47.8%-56.7%, is all better than the function of reducing blood sugar (44.0% and 34.6%) of the Flos Osmanthi Fragrantis polyphenol extract group of same dosage verbascoside group and [201310169455.1].
Table 1 Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract is on the impact of diabetic model rats blood glucose
Note: ▲ represent and compare with Normal group, P<0.01; * represent and compare with model control group, P<0.01; # represents and compares before and after medication, P<0.05; Flos Osmanthi Fragrantis polyphenol extract is for preparing gained according to embodiment 1 in patent of invention [201310169455.1].
Embodiment 6:
Diabetics 342 example, all meets WH0 diabetes diagnostic criterion, wherein man 199 example, female 143 example, 37 ~ 69 years old age, average (51.39 ± 4.72) year, the course of disease 6 ~ 17 years, average (11.07 ± 6.34) year.Be divided into embodiment 1 group of 70 example, embodiment 3 group of 71 example, embodiment 4 group of 64 example, Flos Osmanthi Fragrantis polyphenol extract group 68 example of [201310169455.1], verbascoside 69 example, two groups in sex, age, fasting glucose etc. through statistical procedures there are no significant difference (P > 0.05), there is comparability.Patient's main manifestations is " diabetes ", thirsty polydipsia, polyphagia, urinary micturition, dryness of the mouth and throat, the few tongue of red tongue, stringy pulse.Fasting glucose (10.47 ± 4.51) mmol/L, 2h-plasma glucose (12.67 ± 3.65) mmol/L.
Method is take Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, the verbascoside of embodiment 1,3,4 respectively, in phenylethanoid glycosides 6g/ time, takes Flos Osmanthi Fragrantis polyphenol extract, in total phenols+phenethyl alcohol glycoside 6g/ time, 2 times/day, often organizes and is 8 weeks the course for the treatment of.Announce new " new Chinese medicine guideline of clinical investigations " according to health ministry, effective standard disappears substantially for treating rear symptom, fasting glucose < 7.2mmol/L, 2h-plasma glucose < 8.3mmol/L, or after treatment, blood glucose declines more than 30% before comparatively treating.Effective standard is: after treatment, symptom is obviously improved, fasting glucose < 8.3mmol/L, 2h-plasma glucose < 10.0mmol/L, or after treatment, blood glucose declines more than 10% before comparatively treating.Invalid: after treatment, symptom is not improved, blood glucose declines and does not reach above-mentioned standard.Statistical procedures adopts SPSS20.0 statistical package to carry out date processing and analysis, and measurement data represents with mean ± standard deviation (x ± s), and between group, mean compares and checks with t, and P < 0.05 has statistical significance for difference.After five groups of patient treatments, the total effective rate for the treatment of is respectively 84.29%, 90.04%, 78.12%, 70.58%, 68.1%, the Flos Osmanthi Fragrantis polyphenol extract of verbascoside and [201310169455.1] is better than, in table 2 with dose delivery example 1, embodiment 3 groups, embodiment 4 groups of function of reducing blood sugars.Before and after five groups of treatments, fasting glucose, 2h-plasma glucose compare: after treatment group fasting glucose, after the meal 2 hours blood glucose treatments, all comparatively treatment is front significantly improves, compare before and after treatment, difference has statistical significance (P < 0.05), the Flos Osmanthi Fragrantis polyphenol extract of verbascoside and [201310169455.1] is better than, in table 3 with dose delivery example 1, embodiment 3 groups, embodiment 4 groups of function of reducing blood sugars.
Table 2 Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract is to diabetics comparitive study
Note: Flos Osmanthi Fragrantis polyphenol extract is for preparing gained according to embodiment 1 in patent of invention [201310169455.1].
Table 3 Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract is to empty stomach before and after diabetic therapy and 2h-plasma glucose change
Note: # represents and compares before and after medication, P<0.05; Flos Osmanthi Fragrantis polyphenol extract is for preparing gained according to embodiment 1 in patent of invention [201310169455.1].
Finally, it is also to be noted that what enumerate above is only several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be had.All distortion that those of ordinary skill in the art can directly derive from content disclosed by the invention or associate, all should think protection scope of the present invention.
Claims (5)
1. Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, is characterized in that: in Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract, phenylethanoid glycosides content is 30 ~ 90 % by weight, and described phenylethanoid glycosides comprises verbascoside, different verbascoside;
In phenylethanoid glycosides, verbascoside is 48:1 or 77:1 with the ratio of the weight of different verbascoside.
2. Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract according to claim 1, is characterized in that preparation method is any one method following:
Method one, to comprise the following steps:
(a), the Osmanthus tragranscv.Aurantiacu dry flower of 1kg moisture≤10% is crushed to and can crosses 20 objects sieves, being added to 10L volumetric concentration is in the ethanol water of 90%, add AOB solution 2L again, utilizing 1mol/L acetic acid aqueous solution to adjust pH is 5, obtains extraction solution;
Containing 1g AOB in often liter of AOB solution;
(b), extraction solution is carried out lixiviate 2 hours at 50 ~ 80 DEG C, after being cooled to room temperature, filter or centrifugal, obtain extracting solution;
(c), extracting solution is reclaimed 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 through adsorbent resin, be the ethanol water eluting of 30% by volumetric concentration;
E, after (), eluent concentrating under reduced pressure, spray-dried, low pressure is dried or microwave drying, obtains Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract;
Method two, to comprise the following steps:
(a), the Osmanthus fragrans var.thunbergii. dry flower of 1kg moisture content≤10% is crushed to and can crosses 20 objects sieves, being added to 15L volumetric concentration is in 80% ethanol water, add arabo-ascorbic acid sodium water solution 2L again, utilizing the adjustment of 1mol/L aqueous formic acid to extract pH value of solution is 5, obtains extraction solution;
Containing 1g sodium erythorbate in often liter of arabo-ascorbic acid sodium water solution;
(b), extraction solution is carried out lixiviate 2 hours at 50 ~ 80 DEG C, after being cooled to room temperature, filter or centrifugal, obtain extracting solution;
(c), extracting solution is reclaimed 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 through adsorbent resin, be the ethanol water eluting of 30% by volumetric concentration;
E, after (), eluent concentrating under reduced pressure, spray-dried, low pressure is dried or microwave drying, obtains Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract.
3. utilize Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract as claimed in claim 1 or 2 to prepare and the compositions that obtains, it is characterized in that: described combination species contain the Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract of 0.01 ~ 99.9wt%, surplus is carrier.
4. compositions according to claim 3, is characterized in that: compositions is pharmaceutical composition, Halth-care composition, food compositions or cosmetic composition.
5. the purposes of Flos Osmanthi Fragrantis phenethyl alcohol glycoside extract as claimed in claim 1 or 2, is characterized in that: for the preparation of preventing and treating the food of diabetes, medicine or health product.
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| CN104231011B (en) * | 2014-09-12 | 2017-02-15 | 苏州禾研生物技术有限公司 | Preparation method of verbascoside |
| CN105832603A (en) * | 2016-04-22 | 2016-08-10 | 无限极（中国）有限公司 | Preparation method and application of sweet-scented osmanthus extract |
| 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 |
| CN107998183B (en) * | 2017-12-26 | 2021-05-04 | 浙江大学 | Osmanthus fragrans phenylethanoid glycoside liposome coated with chitosan and preparation method thereof |
| 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 |
| CN113398030A (en) * | 2021-07-09 | 2021-09-17 | 广州集妍化妆品科技有限公司 | Osmanthus fragrans flower extract, preparation method thereof and cosmetic |
| CN115368421B (en) * | 2022-10-21 | 2023-01-03 | 中国科学院华南植物园 | Method for preparing phenylethanoid glycosides compounds by using michelia plants |
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