CN107823188A - A kind of compound flavones spansule and preparation method thereof - Google Patents
A kind of compound flavones spansule and preparation method thereof Download PDFInfo
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- CN107823188A CN107823188A CN201711185163.1A CN201711185163A CN107823188A CN 107823188 A CN107823188 A CN 107823188A CN 201711185163 A CN201711185163 A CN 201711185163A CN 107823188 A CN107823188 A CN 107823188A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/54—Lauraceae (Laurel family), e.g. cinnamon or sassafras
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1629—Organic macromolecular compounds
- A61K9/1652—Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
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Abstract
A kind of compound flavones spansule of disclosure of the invention and preparation method thereof, using the method for beta cyclodextrin Laoyin tea flavones inclusion compound slow-release capsules, prepare inclusion compound, saturated aqueous solution is made in beta cyclodextrin, it is then gradually adding the hydrothermal solution of Laoyin tea chromocor extract, reduced vacuum is dried, and solid crushes to obtain inclusion compound；Prepare slow-releasing granules：By ethyl cellulose, HPMC and obtained inclusion compound, it is placed in drying receptacle and mixes, add ethanol solution, stirs to solid-state like, dry, pulverize, obtain particle.Invention increases solubility in the water of flavones in Laoyin tea, improves Laoyin tea flavones Bioavailability of Human Body, improves health-care effect timeliness.Compared with prior art, blood sugar decreasing effect is obvious after adhering to eating compound flavones spansule of the invention for a period of time, can control the blood sugar level of diabetic and the hazards of correlation, and then improve the life quality of diabetic.
Description
Technical field
The invention belongs to field of pharmaceutical technology, and in particular to a kind of compound flavones spansule and preparation method thereof.
Background technology
Laoyin tea contains the compositions such as flavones, glycoside, organic acid, cumarin and tannin, and wherein flavonoids is the master of Laoyin tea
Composition is wanted, mainly there is Kaempferol, Kaempferol-glucose villous themeda and Quercetin-glucoside.Result of study shows that Laoyin tea can reduce
The blood-sugar content of normal mouse, prompt it can be by stimulating the cells secrete insulin of pancreas islet 13 to produce blood sugar reducing function.Adrenaline
Make blood glucose rise by decomposing hepatic glycogen, and Laoyin tea reduces the blood glucose value of adrenaline-induced hyperglycosemia rats, illustrates that it may
There is to suppress hepatic glycogenolytic caused by adrenaline and promote hepatic glycogen synthesis, so as to reduce the source of blood glucose, increase
Heal the outlet of sugar, hence it is evident that reduce blood glucose rise caused by metabolic disorder.Alloxan and Streptozotocin are B cell
Agent is killed, optionally impaired isle B cell, causes artificial diabetes.In diabetic mice and rat model, eagle
Tea has significant blood sugar reducing function, while the release to insulin in alloxan diabetes mice serum also there is promotion to make
With.Prompt it mainly by protecting pancreas islet p cells or promoting reparation and promotion insulin secretion, the increase blood of impaired mouth cells
Clear insulin content and reach the purpose for reducing blood glucose.
(β-Cyclodextrin's beta-schardinger dextrin abridge：β-CD) it is that the ring that starch is obtained by culture with alkaline bacillus is pasted
The product formed after smart glucan indexing enzyme effect.β-CD are the crystalline powders of white, by 7 glucose units through α-Isosorbide-5-Nitrae
Sugared key connection circularizes structure, annular in shape hollow cartridge type, has special construction hydrophobic in hydrophilic, ring outside ring and property.Its ring
Shape structure can enter cyclodextrin cavity with hydrophobic interior cavities with inclusion difference compound, guest molecule, due to the change of microenvironment,
Significant change occurs for its physicochemical properties.Under room temperature condition, the solubility in water is 1.85g/100ml.β-CD itself do not have
Toxic side effect, therefore, cyclodextrin one of the aspect being utilized that takes the lead in is exactly drug field；β-CD surface-actives are low, hemolytic activity
Low, use is safer.Experiment shows that β-CD traditional Chinese medicine inclusion compounds can improve the stability of active compound thing；Prevent oxidation of drug, decompose；
Improve drug solubility and bioavilability；Reduce the Side effect of medicine.All these advantages are obviously processed to Chinese medicine
Industry and food, health products trade are all highly useful, you can so that formulation is improved, can strengthen drug absorption again, may be used also
To improve medicine mouthfeel, and β-CD are sugar-free composition, are applicable to the patients such as diabetes, high fat of blood, obesity.
Diabetes are a kind of common multiple metabolic diseases, are often accompanied by the rise of blood fat, and glucose-lipid metabolism is disorderly and glycosuria
The occurrence and development of sick chronic complicating diseases are closely related.Therefore blood fat is reduced for preventing or delaying complication, improve patient of diabetes
The prognosis of person is significant.Capillary Electrophoresis (Capillary electrophoresis, CE) is a kind of efficient, quick
With the isolation technics of low consumption, it is especially suitable for separating some and does not retain on HPLC or be difficult to the composition analyzed, and sample is pre-
Handle infringement problem that is relatively simple, or even being not required to consider post, the organic acid compound available for measure plant.For
The common organic acid compound without ultraviolet absorption group, typically surveyed using indirect ultraviolet method (indirect UV, IUV)
Fixed, CE-IUV measure organic acid compounds are a kind of fast and convenient methods.Laoyin tea (Litsea coreana Level)
Also known as Litsea coreana, white tea is commonly called as, is distributed in the ground such as Sichuan, Guizhou, Yunnan, Anhui, is south China various nationalities long-term drink among the people
A kind of plant alternative tea, there is removing toxicity for detumescence, improving eyesight benefit to think, promote the production of body fluid to quench thirst, inducing diaphoresis heatstroke prevention and other effects.Herein with 4,5-miaow
Azoles dicarboxylic acids (4,5-imidazolecarboxylic acid, IDC) is back-ground electolyte, is established a kind of quick, sensitive
The CE-IUV methods of organic acid compound are analyzed, the method is also applied to 7 kinds of organic acid compounds and flavones in Laoyin tea
Analysis.
The present invention is back-ground electolyte using 4,5- imidazole-2-carboxylic acids (IDC), with 20mmol/L IDC-0.5mmol/L ten
Six alkyl trimethyl ammonium bromides (cetytrimethylammonium bromide, CTAB) electrophoresis solution (pH 12.1), separation
Voltage is -30kV, column temperature is 20 DEG C, long capillary tube 95cm, seven kinds of organic acid chemical combination in separation determination Laoyin tea and ginkgo
The content of thing (oxalic acid, formic acid, citric acid, malic acid, Cys, Pidolidone and acetic acid) and flavones, this method simplicity,
Quickly, accurately.
The content of the invention
The invention provides a kind of compound flavones spansule and preparation method thereof, it is characterised in that methods described is by as follows
Step is carried out：
1) preparation of inclusion compound：In stainless ceramic reactor, in 50 DEG C~70 DEG C of chuck bath temperature, agitator speed
Under conditions of 120~180 revs/min, saturated aqueous solution is made in the beta-schardinger dextrin of 8~12 parts by weight, is then gradually adding 2.8
The hydrothermal solution of the Laoyin tea chromocor extract of~4.2 parts by weight, is stirred 2~3h, stands 8~15h at room temperature, filters,
Filtered fluid is concentrated into 1/3 volume, and 50 DEG C~70 DEG C reduced vacuums are dried, and solid crushes to obtain beta-schardinger dextrin Laoyin tea flavones inclusion
Thing；
2) preparation of slow-releasing granules：The ethyl cellulose of 20~50 parts by weight, 0.87~2.3 parts by weight hydroxypropyl is fine
Inclusion compound made from the steps 1) of dimension element and 8~23 parts by weight, is placed in drying receptacle and mixes, add ethanol solution, and 50 DEG C~60
DEG C circulating water heating, makes mixture complete miscibility, stirs to solid-state like, dry, pulverize at 60 DEG C~90 DEG C, obtain particle；
3) spansule is filling：By above-mentioned steps 2) granule filling capsulae vacuus is made, obtain beta-schardinger dextrin Laoyin tea Huang
Ketone inclusion compound slow-release capsules.
As preferred means, general flavone content is 60.2% in Laoyin tea chromocor extract in step 1), in 60 DEG C of decompressions
Vacuum drying, the ethanol solution concentration of addition is 95%.
As preferred means, in step 1), Laoyin tea flavones is extracted, purifying, concentration and obtain brown powder extract.
It as preferred means, in step 2), dry, pulverize at 80 DEG C, cross 20 mesh sieves, fine powder is removed with 60 mesh sieves, obtain
Grain.
As preferred means, beta-schardinger dextrin used, ethyl cellulose, HPMC are food-grade in step 2)
Raw material or pharmaceutical grade raw material.
As further preferred means, Capillary Electrophoresis-indirect ultraviolet method using IDC as back-ground electolyte determines compound
The content of organic acid and flavones in flavones product.Carry out as follows：Laoyin tea-GINKGO BILOBA EXTRACT crude extract precision is measured
2ml, mixed with equivalent 2ml acetonitriles, strength shakes, and takes appropriate solution to centrifuge 10min, supernatant in 10000rpm rotating speeds after standing
With 0.45 μm of membrane filtration, then appropriate dilution or direct injected measure.
Embodiment
The linear relationship of embodiment 1. is investigated
Laoyin tea-GINKGO BILOBA EXTRACT crude extract of serial various concentrations is taken, is determined by the following procedure：
Quartz capillary is cleaned with 1mol/L hydrochloric acid, water, 1mol/L sodium hydroxides and water successively before using daily, is finally used
Buffer solution balances 10min.Electrophoresis interval uses wash buffer 10min twice, and buffer solution after 4 times using changing.Running buffer is molten
Liquid：20mmol/L IDC -0.5mmol/L CTAB (pH 12.1), capillary column：95cm × 75 μm, coolant temperature：20 DEG C,
Sample introduction：0.5psi × 5s, separation voltage：- 30kV, Detection wavelength：214nm.
Be ordinate with peak area (A), reference substance concentration (C, μ g/mL) be that abscissa draws standard curve, obtain linear
Regression equation and the range of linearity, oxalic acid, formic acid, the range of linearity of Pidolidone and acetic acid are 20-1000 μ g/mL, citric acid and
The range of linearity of malic acid is 20-500 μ g/mL, and the range of linearity of Cys is 50-1000 μ g/mL.According to 3 times of noises
Detection limit, oxalic acid, formic acid, citric acid, malic acid, Pidolidone and acetic acid, the line of flavones are determined than (S/N=3) corresponding concentration
Sexual intercourse and detection limit the results are shown in Table 1.
The linear relationship of organic acid and flavones, detection limit in the compound sustained release capsules of table 1.
The precision test of embodiment 2.
200 μ g/ml mixed reference substance solutions are taken, according to the assay method of embodiment 1, METHOD FOR CONTINUOUS DETERMINATION 6 times, calculating 7 kinds has
The peak area relative standard deviation (RSD) of machine acid and flavones, as a result oxalic acid, formic acid, citric acid, malic acid, Cys, L-
The peak area RSD of glutamic acid, acetic acid and flavones is respectively 1.98%, 1.97%, 1.82%, 2.02%, 2.05%, 1.91%,
1.63%, 6.55%, show that this method precision is good.
The replica test of embodiment 3.
1.0g Laoyin teas -6 parts of ginkgo sample is weighed respectively, it is accurately weighed, sample solution, measure 7 are prepared as follows
The peak area of kind organic acid：
Laoyin tea-ginkgo sample is put in vacuum drying chamber dries 4h in 60 DEG C, 40 mesh sieves is crossed after grinding, precision weighs fine powder
About 1.0g, it is placed in band plug conical flask, adds 10ml water, ultrasonic 1h, stand, filtering, with 5ml water washing residues, merging filtrate, water
It is placed in after bath concentration in 10ml measuring bottles, adds water to scale, shake up, precision measures 2ml sample solutions, is mixed with equivalent 2ml acetonitriles,
Strength shakes, and takes appropriate solution to centrifuge 10min, 0.45 μm of membrane filtration of supernatant in 10000rpm rotating speeds after standing, then fit
When dilution or direct injected measure.
As a result the peak area RSD of oxalic acid, formic acid, citric acid, malic acid, Cys, Pidolidone, acetic acid and flavones
Respectively 2.05%, 2.08%, 2.03%, 2.05%, 2.04%, 2.01%, 1.76%, 6.37%, show that the method repeats
Property is good.
The stability test of embodiment 4.
Sample solution is prepared as described in Example 3, it is organic respectively at 0,3,6,12,24h sample introductions are postponed, recording 7 kinds
The peak area RSD of sour peak area, as a result oxalic acid, formic acid, citric acid, malic acid, Cys, glutamic acid, acetic acid and flavones
Respectively 2.15%, 2.12%, 2.14%, 2.17%, 2.01%, 2.02%, 1.67%, 6.38%, show this method in 24h
Interior stabilization.
It can be seen that from above example result and use IDC as back-ground electolyte, with CTAB electrophoresis solution split-voltages
Seven kinds of organic acid compounds (oxalic acid, formic acid, citric acid, malic acid, Guangs of L- half in the Laoyin tea of measure-ginkgo spansule
Propylhomoserin, Pidolidone and acetic acid) and flavones content, this method method is easy, quick, accurate, and preparation method operation letter
It is single, it is relatively low without special installation, short preparation period, cost without sterilization steps.
The description to embodiment the invention is not restricted to more than, those skilled in the art according to disclosure of the present invention,
The creative work improvement and modification that be carried out need not be passed through on the basis of the present invention, all should protection scope of the present invention it
It is interior.
Claims (7)
1. a kind of compound flavones spansule and preparation method thereof, it is characterised in that this method comprises the following steps：
1) preparation of inclusion compound：In stainless ceramic reactor, it is in 50 DEG C~70 DEG C of chuck bath temperature, agitator speed
Under conditions of 120~180 revs/min, saturated aqueous solution is made in the beta-schardinger dextrin of 8~12 parts by weight, it is then gradually adding 2.8~
The hydrothermal solution of the Laoyin tea chromocor extract of 4.2 parts by weight, is stirred 2~3h, stands 8~15h, filtering, mistake at room temperature
Filtrate is concentrated into 1/3 volume, and 50 DEG C~70 DEG C reduced vacuums are dried, and solid crushes to obtain beta-schardinger dextrin Laoyin tea flavones inclusion
Thing；
2) preparation of slow-releasing granules：By the ethyl cellulose of 20~50 parts by weight, 0.87~2.3 parts by weight HPMC
And 8~23 parts by weight step 1) made from inclusion compound, be placed in drying receptacle and mix, add ethanol solution, 50 DEG C~60 DEG C are followed
Ring water heats, and makes mixture complete miscibility, stirs to solid-state like, dry, pulverize at 60 DEG C~90 DEG C, obtain particle；
3) spansule is filling：By above-mentioned steps 2) granule filling capsulae vacuus is made, obtain beta-schardinger dextrin Laoyin tea flavones bag
Compound spansule；
4) Capillary Electrophoresis-indirect ultraviolet method using IDC as back-ground electolyte determines organic acid and flavones in compound flavones product
Content.
2. the preparation method of beta-schardinger dextrin Laoyin tea flavones inclusion compound slow-release capsules according to claim 1, its feature exist
In：In step 1), general flavone content is 60.2% in Laoyin tea chromocor extract.
3. the preparation method of beta-schardinger dextrin Laoyin tea flavones inclusion compound slow-release capsules according to claim 1, its feature exist
In：In step 1), dried in 60 DEG C of reduced vacuums.
4. the preparation method of beta-schardinger dextrin Laoyin tea flavones inclusion compound slow-release capsules according to claim 1, its feature exist
In：In step 2), the ethanol solution concentration of addition is 95%.
5. the preparation method of beta-schardinger dextrin Laoyin tea flavones inclusion compound slow-release capsules according to claim 1, its feature exist
In：It in step 2), dry, pulverize at 80 DEG C, cross 20 mesh sieves, remove fine powder with 60 mesh sieves, obtain particle.
6. the preparation method of beta-schardinger dextrin Laoyin tea flavones inclusion compound slow-release capsules according to claim 1, its feature exist
In：Beta-schardinger dextrin used, ethyl cellulose, HPMC are food grade materials or pharmaceutical grade raw material in step 2).
7. the preparation method of beta-schardinger dextrin Laoyin tea flavones inclusion compound slow-release capsules according to claim 1, its feature exist
In：In step 1), Laoyin tea flavones is extracted, purifies, concentration, obtains brown powder extract.
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| CN201711185163.1A CN107823188A (en) | 2017-11-23 | 2017-11-23 | A kind of compound flavones spansule and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115038340A (en) * | 2019-12-16 | 2022-09-09 | 昊福食品私人有限公司 | Preparation, composition or food additive for changing blood sugar reaction, and its preparation method and application |
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2017
- 2017-11-23 CN CN201711185163.1A patent/CN107823188A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115038340A (en) * | 2019-12-16 | 2022-09-09 | 昊福食品私人有限公司 | Preparation, composition or food additive for changing blood sugar reaction, and its preparation method and application |
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Application publication date: 20180323 |