CN106963807B - A kind of hypoglycemic oral liquid and preparation method thereof - Google Patents
A kind of hypoglycemic oral liquid and preparation method thereof Download PDFInfo
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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)
- A61K36/52—Juglandaceae (Walnut family)
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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)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
- A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
- A61K47/12—Carboxylic acids; Salts or anhydrides thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
- A61K47/20—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing sulfur, e.g. dimethyl sulfoxide [DMSO], docusate, sodium lauryl sulfate or aminosulfonic acids
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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
- A61K9/0012—Galenical forms characterised by the site of application
- A61K9/0053—Mouth and digestive tract, i.e. intraoral and peroral administration
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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
- A61K9/08—Solutions
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Abstract
The present invention discloses a kind of hypoglycemic oral liquid, by weight, include blue or green money willow polysaccharide 15~30%, blue or green money willow chromocor extract 2~4%, maniod ebish flower extract 15~40%, ZTC1+1 natural clarifying agents 4~6%, sodium benzoate 0.4~0.6%, honey element 0.1~0.2%, glycerine 0.8~1.5%, remaining is water, and raw material summation is 100%；Preparation method mixes blue or green money willow polysaccharide, chromocor extract, maniod ebish flower extract, ZTC1+1 natural clarifying agents, sodium benzoate, honey element, G ＆ W, through 200 mesh sieve net filtrations, after filling and capping, with 100~120 DEG C of 10~30min of sterilization, room temperature is cooled to, labeling, outer packing obtain product.Oral liquid for decreasing blood sugar is made in Qingqian Willow leaf blood-sugar-lowering effective parts extract compatibility maniod ebish flower extract by the present invention, improves the hypoglycemic bioavilability of Qingqian Willow leaf, is played multiple medicine and is cooperateed with hypoglycemic effect.
Description
Technical field
The present invention relates to a kind of hypoglycemic oral liquid and preparation method thereof, belong to technical field of health care food.
Background technology
In recent years, China's diabetes prevalence is gradually increasing, and treats diabetes at present mainly by OHA and pancreas islet
Element.But often there are the adverse reactions such as hypoglycemia and gastrointestinal discomfort in Western medicine；And treatment by Chinese herbs has curative effect stabilization, side effect
The characteristics of small, Mutiple Targets act on simultaneously, the treatment of suitable diabetes and its complication.
Blue or green money willow (Cyclocaryapaliurus (Bata1) Iljinsk) is Juglandaceae cyclocarya deciduous tree, Jiangxi
It is among the people to be drunk for a long time using its tender leaf tea making, the tea have promote the production of body fluid to quench thirst, clearing away summerheat, hypoglycemic, reducing blood lipid, drop blood
Press and the effect such as promote longevity, flavonoids, polysaccharide and the trace element in blue or green money willow have preferable hypoglycemic effect.It is blue or green at present
Money willow hypoglycemic product mainly has the solid pharmaceutical preparations such as blue or green money willow tea bag, buccal tablet, and it is directly brewed for for Qingqian Willow leaf or blue or green money
Willow crude extract preparation, active ingredient being present, absorptivity is low in vivo, soak time is long, takes the shortcomings of inconvenience.
The content of the invention
In view of the above-mentioned problems of the prior art, the present invention provides a kind of hypoglycemic oral liquid and preparation method thereof, carry
The high hypoglycemic bioavilability of Qingqian Willow leaf, play multiple medicine and cooperate with hypoglycemic effect, so as to improve the hypoglycemic of whole preparation effect
Fruit.
To achieve these goals, a kind of hypoglycemic oral liquid that the present invention uses, the raw material comprising following weight ratio：It is blue or green
Money willow polysaccharide 15~30%, blue or green money willow chromocor extract 2~4%, maniod ebish flower extract 15~40%, ZTC1+1 natural clears
Agent 4~6%, sodium benzoate 0.4~0.6%, honey element 0.1~0.2%, glycerine 0.8~1.5%, remaining is water, raw material summation
For 100%.
As an improvement, each material rate is according to containing blue or green money willow polysaccharide 1.54g, blue or green money willow extracting flavonoids in 10ml oral liquids
Thing 0.235g, maniod ebish flower extract 1.9g, ZTC1+1 natural clarifying agent 0.6ml, sodium benzoate 0.04g, honey element 0.02g,
Glycerine 0.15ml, surplus are water.
In addition, present invention also offers a kind of preparation method of hypoglycemic oral liquid, by blue or green money willow polysaccharide, blue or green money willow flavones
Extract, maniod ebish flower extract, ZTC1+1 natural clarifying agents, sodium benzoate, honey element, G ＆ W mixing, through 200 mesh sieves
Net filtration, after filling, capping, using 100~120 DEG C of 10~30min of sterilization, room temperature is cooled to, labeling, outer packing obtain product.
As an improvement, the blue or green money willow chromocor extract and blue or green money willow polysaccharide are made by following steps respectively：
1) take blue or green money willow dried leaf to crush, add water to cook three times, merging filtrate, filtering, concentration, absolute ethyl alcohol is added after cooling
To alcohol content up to 65%, place 24 hours, filtering, filtrate is standby respectively with precipitation；
2) after macroporous absorbent resin pretreatment, upper macroporous absorption after the rotated evaporimeter concentration of filtrate that step 1) is obtained
Resin column, after adsorbing 5 hours, macroreticular resin is rushed with water, 60% ethanol, 85% ethanol, 95% ethanol respectively, collects eluent,
Merge after thin-layer chromatography point plate, concentrated with Rotary Evaporators, dried after reclaiming ethanol, produce blue or green money willow chromocor extract；
3) precipitation that step 1) obtains is concentrated with Rotary Evaporators, reclaims ethanol, its volume 1/5 is added into concentrate
Chloroform and 1/5 n-butanol, shake 30min, the mixed liquor after concussion centrifuges 10min under 2000r/min rotating speed, takes out
Supernatant, repeats above step 5 times, removes organic solvent portion and protein portion, obtains refined blue or green money willow polysaccharide.
As an improvement, the maniod ebish flower extract is adopted and is prepared by the following steps：Sunset abelmoschus flower crushes, and adds ethanol to decoct three
Time, merging filtrate, concentrated after filtering and produce maniod ebish flower extract.
As an improvement, the ZTC1+1 natural clarifying agents are adopted and are prepared by the following steps：Component A and B component are each configured to
1% viscose, first plus after B add A, standing 6-12 hours produce.
Compared with prior art, it is of the invention by the hypoglycemic medicinal plant of Qingqian Willow leaf blood-sugar-lowering effective parts extract compatibility
Maniod ebish flower extract is prepared into oral liquid for decreasing blood sugar, has both improved the hypoglycemic bioavilability of Qingqian Willow leaf, plays multiple medicine association again
With hypoglycemic effect, so as to improve the hypoglycemic effect of whole preparation.
Brief description of the drawings
Fig. 1 is blue or green money willow chromocor extract, the extraction process flow chart of blue or green money willow polysaccharide in the present invention；
Fig. 2 is the glucose standard curve that the present invention is drawn；
Fig. 3 is the pancreatic tissue cells figure of blank control group；
Fig. 4 is the pancreas after oral liquid (blue or green money willow polysaccharide+blue or green money willow flavones+maniod ebish flower extract) middle dosage (100 ×)
Glandular tissue cytological map；
Fig. 5 is the pancreatic tissue cells figure of model group (100 ×)；
Fig. 6 is the pancreatic tissue cells figure of diabetes pill group (100 ×).
Embodiment
To make the object, technical solutions and advantages of the present invention of greater clarity, below by drawings and Examples, to this
Invention is further elaborated.However, it should be understood that the specific embodiments described herein are merely illustrative of the present invention,
The scope being not intended to limit the invention.
Unless otherwise defined, all technical terms and scientific terminology used herein are led with belonging to the technology of the present invention
The implication that the technical staff in domain is generally understood that is identical, and used term is intended merely to retouch in the description of the invention herein
State the purpose of specific embodiment, it is not intended that in the limitation present invention.
Embodiment one
1. the extraction separation of blue or green money willow chromocor extract, blue or green money willow polysaccharide and maniod ebish flower extract.
1.1 raw materials and reagent
Qingqian Willow leaf：In June, 2013 picks up from xiushui；
Sunset abelmoschus flower：Pick up from Anhui inaction in June, 2013；
Rutin standard items；Glucose；Phenol；The concentrated sulfuric acid；
Absolute ethyl alcohol：Wuxi City Su Qiang Chemical Co., Ltd.s；
Sodium hydroxide：Tianjin Kermel Chemical Reagent Co., Ltd.；
Hydrochloric acid；Chloroform；N-butanol；Methanol；
1.2 instrument and equipment
Pulverizer (RHP-400A types)：Zhejiang Yongkang City Rong Hao Trade Co., Ltd.s；
D101 macroporous absorbent resins：Hangzhou Pu Xiu bio tech ltd；
Rotary Evaporators (N1100)：Shanghai Ai Lang Instrument Ltd；
Digital display temperature controlled water bath pot：Upper hypo Lip river experimental facilities Co., Ltd；
Digital display air dry oven (GZX-9246)：Shanghai Medical Equipment Plant of Bo Yuan Industrial Co., Ltd.s；
Section's life board Medical ultrasonic cleaner (KS-600D)：Ningbo Hai Shu Ke Sheng ultrasonic devices Co., Ltd；
Large Copacity centrifuge (XYJ-A2)：Jintan City city east Xin Rui instrument plants；
Electronic balance (ACS-30)：Yongkang City You Sheng weighing apparatus Co., Ltd manufactures；Electromagnetic oven；
TU-1900 dual-beams ultraviolet-uisible spectrophotometer (Beijing Pu Xi all purpose instruments Co., Ltd)；
UV-2000 types ultraviolet-uisible spectrophotometer (outstanding Nico Shanghai Instrument Ltd.)；
Shaking table；Humidifier；Tool plug test tube；Volumetric flask；
The extraction of 1.3 blue or green money willow chromocor extracts, blue or green money willow polysaccharide, its technique are as shown in Figure 1：
1.3.1 water extraction and alcohol precipitation method
Step：Qingqian Willow leaf is crushed → added water to cook three times, merging filtrate → filtering → concentration, cooling → plus absolute ethyl alcohol
It is standby respectively to alcohol content up to 65% → placement 24 hours, filtering, filtrate and precipitation.
1.3.2 macroreticular resin absorbing method Refined flavonoid powder
After macroporous absorbent resin pretreatment, upper macroporous absorption after the rotated evaporimeter of filtrate that upper step tests to obtain is concentrated
Resin column, after adsorbing five hours, macroreticular resin is rushed with water, 60% ethanol, 85% ethanol, 95% ethanol respectively, collects elution
Liquid, merge after thin-layer chromatography point plate, concentrated with Rotary Evaporators, after reclaiming ethanol, obtain dry total flavone part.
1.3.3 the measure of flavones content：Ultraviolet spectrophotometry
(1) step：
1. rutin standard liquid：Weigh and the control substance of Rutin 5.5mg to constant weight dried at 120 DEG C in 50mL volumetric flasks,
Scale is settled to the dissolving of 70% ethanol, is shaken up, as reference substance solution (containing rutin 0.11mg per 1mL).
2. configure blue or green money willow general flavone liquid with method：Dried general flavone 5.5mg is weighed in 50mL volumetric flasks, constant volume,
Shake up and (contain general flavone 0.11mg per 1mL).
3. blue or green money willow general flavone liquid, each 1mL of control substance of Rutin solution are taken respectively in 10mL tool plug test tubes, ethanol constant volume,
Shake up, be scanned after 10min with dual-beam ultraviolet specrophotometer in 200~450nm wave-length coverages, ethanol makees blank
Liquid.
(2) result：The content of flavones is 75% in obtained Qingqian Willow leaf general flavone.
1.3.4Sevage method refined polysaccharide
(1) step：
1. the precipitation that upper step is tested to obtain is concentrated with Rotary Evaporators, ethanol is reclaimed；
2. adding the chloroform of its volume 1/5 and 1/5 n-butanol into concentrate, 30min, the mixed liquor after concussion are shaken
10min is centrifuged under 2000r/min rotating speed；Supernatant is taken out, repeats above step 5 times；
3. removing organic solvent portion and protein portion, refined blue or green money willow polysaccharide is obtained.
(2) phenomenon and conclusion
1. there is gelling material generation, water layer and solvent layer intersection are denatured protein.
2. remove organic solvent portion and protein portion, you can obtain Deproteinated polysaccharide solution.
1.3.5 measurement of the polysaccharide content：Sulfuric acid-phynol method
(1) step：
1. the drafting of glucose standard curve：Take glucose 100g to dry to constant weight, accurately weigh 209.2mg, put 200mL
In volumetric flask, it is dissolved in water and is diluted to scale, obtains the standard liquid that concentration is 1.046mg/mL, draw glucose standards solution
0.1st, 0.2,0.4,0.6,0.8mL, puts in 100mL volumetric flasks, adds water constant volume, respectively draw 2mL, be respectively placed in colorimetric cylinder respectively
In, add 5% phenol liquid 1mL, shake up, it is rapid that concentrated sulfuric acid 5mL is added dropwise, shake up, 20min is heated in boiling water bath, be rapidly cooled to
Room temperature, separately with distilled water 2mL, ibid operation plus phenol and sulfuric acid progress chromogenic reaction, make blank control, determine absorbance, paint
Standard curve processed, calculate regression equation.
2. the configuration of blue or green money willow polysaccharide solution：Dried polysaccharide 5.0mg is weighed in 50mL volumetric flasks, constant volume, is shaken up
(containing Thick many candies 0.1mg per 1mL).
3. measurement of the polysaccharide content：
Taking blue or green money willow polysaccharide liquid 0.5ml, → addition 1.5ml distilled water → takes 5% phenol 1ml → concentrated sulfuric acid 5ml → to shake
It is even, 20min → room temperature natural cooling in 100 DEG C of boiling water baths → OD is surveyed at wavelength 488nm.
4. glucose standard curve：Using dextrose standard sample concentration as abscissa, absorbance is ordinate, makees standard curve
(such as Fig. 2), regression equation is sought, the regression equation of standard curve is that (wherein Y is absorbance to Y=5.4407c+0.0253, and c is
Concentration of glucose), R^2=0.9990.
(2) result：The content of polysaccharide is about 27% in total starches in Qingqian Willow leaf.
1.3.6 result is with discussing
By water extraction and alcohol precipitation method, macroreticular resin absorbing method is refined and Sevage methods obtain blue or green money willow general flavone and Thick many candies.
The content that ultraviolet spectrophotometry and sulfuric acid-phynol method measure flavones in Qingqian Willow leaf general flavone respectively is 75%, in total starches
The content 27% of polysaccharide.
The extraction separation of 1.4 maniod ebish flower extracts
Step：Sunset abelmoschus flower crushes → added ethanol and decocts three times, and merging filtrate → filtering → concentration is standby.
Embodiment two
1. the preparation of the hypoglycemic oral liquid of blue or green money willow
1.1 raw material and reagent
Blue or green money willow extract solution：Flavones liquid, polysaccharide liquid, sunset abelmoschus flower extract solution；
Fining agent：101 fruit juice clarifiers (talcum powder), ZTC1+1 natural clarifying agents, gelatin-tannic acid；
Preservative：Sodium benzoate；Flavouring：Honey element；Solubilizer：Glycerine；
Glacial acetic acid：Tianjin good fortune morning chemical reagent factory；Glycerine：Tianjin good fortune morning chemical reagent factory；
Rutin standard items；Glucose；Phenol；The concentrated sulfuric acid；Absolute ethyl alcohol；Absolute methanol；
1.2 instrument and equipment
Large Copacity centrifuge (XYJ-A2)：Jintan City city east Xin Rui instrument plants；
Digital display air dry oven (GZX-9246)：Shanghai Medical Equipment Plant of Bo Yuan Industrial Co., Ltd.s；
Digital display temperature controlled water bath pot (upper hypo Lip river experimental facilities Co., Ltd)；
Micropipettor (10-1000 μ L) (Zhejiang Hua Wei scientific instrument Co., Ltd)；
Electronic analytical balance (FA2004)：Shanghai Yue Ping scientific instrument Co., Ltd；
TU-1900 dual-beams ultraviolet-uisible spectrophotometer (Beijing Pu Xi all purpose instruments Co., Ltd)；
UV-2000 types ultraviolet-uisible spectrophotometer (outstanding Nico Shanghai Instrument Ltd.)；
Shaking table；Humidifier；Tool plug test tube；
The various parameters of 1.3 technical schemes of the present invention are with following experimental data and analysis for foundation：
1.3.1 additives screen preliminary experiment
(1) configuration of fining agent and step：
1. 101 fruit juice clarifiers：Concentration 5%, dosage are the 9% of decoction, add 0.5% talcum powder.
2. ZTC1+1 natural clarifying agents：Component A and B component are each configured to 1% viscose, dosage 5%, first plus after B add
A, stand 6-12 hours.
3. gelatin-tannic acid：Dosage is 2%, 50 DEG C of optimum temperature, stands more than 40min.
(2) experimental result：
Through experiment, it was found that, it is best to the addition of the decoction clarity of ZTC1+1 natural clarifying agents, still select ZTC1+
1 natural clarifying agent is as fining agent.Conventional preservative has sodium benzoate and sodium sorbate, and we have found benzene by bacteriostatic experiment
The antiseptic effect of sodium formate is more preferable.It is adapted to the flavouring of diabetic to have honey element and stevioside, we are by orally tasting
The methods of, it is found that honey element is more suitable for.Conventional solubilizer such as sapn, tween etc. have peculiar smell, are not suitable for oral formulations solubilising,
Appropriate medical glycerine solubilising is added in oral liquid, clarity can be improved, and glycerine is sweet, free from extraneous odour, nonirritant.
1.3.2 the preparation technology of oral liquid investigates
Quality and stability and its of oral liquid be formulated in fining agent, preservative, flavouring, solubilizer it is closely related.
Therefore fining agent, preservative, flavouring, solubilizer are investigated respectively by orthogonal test to the principle active component content of oral liquid
Influence, it is determined that optimal preparation technology.
Orthogonal：On the basis of trial test, each factor level value is determined, using the content of active ingredient as investigation
Index, carries out Orthogonal Experiment and Design, and empirical factor level is shown in Table 1.
The preparation technology factor level table of the oral liquid of table 1
1.3.3 oral liquid assay
1.3.3.1 the measure of flavones content：Ultraviolet spectrophotometry
1. rutin standard liquid：Weigh and the control substance of Rutin 5.5mg to constant weight dried at 120 DEG C in 50mL volumetric flasks,
Scale is settled to the dissolving of 70% ethanol, is shaken up, as reference substance solution (containing rutin 0.11mg per 1mL).
2. taking blue or green money willow Sunset Abelmoschus Root oral liquid, each 1mL of control substance of Rutin solution respectively, methanol is fixed in 10mL tool plug test tubes
Hold, shake up, be scanned after 10min with dual-beam ultraviolet specrophotometer in 200~450nm wave-length coverages, methanol is made empty
White liquor.
1.3.3.2 measurement of the polysaccharide content：Sulfuric acid-phynol method
1. the drafting of glucose standard curve：Take glucose 100g to dry to constant weight, accurately weigh 209.2mg, put 200mL
In volumetric flask, it is dissolved in water and is diluted to scale, obtains the standard liquid that concentration is 1.046mg/mL, draw glucose standards solution
0.1st, 0.2,0.4,0.6,0.8mL, puts in 100mL volumetric flasks, adds water constant volume, respectively draw 2mL, be respectively placed in colorimetric cylinder respectively
In, add 5% phenol liquid 1mL, shake up, it is rapid that concentrated sulfuric acid 5mL is added dropwise, shake up, 20min is heated in boiling water bath, be rapidly cooled to
Room temperature, separately with distilled water 2mL, ibid operation plus phenol and sulfuric acid progress chromogenic reaction, make blank control, determine absorbance, paint
Standard curve processed, calculate regression equation.
2. measurement of the polysaccharide content：
Take oral liquid 1ml → constant volume, 100 times of dilution → take dilution 0.5ml → addition 1.5ml distilled water → to take 5%
Phenol 1ml → concentrated sulfuric acid 5ml → shakes up, 20min → room temperature natural cooling in 100 DEG C of boiling water baths → OD is surveyed at wavelength 488nm.
1.3.4 orthogonal experiment and result
Using the content of flavones in oral liquid and polysaccharide as inspection target, L is selected9(34) orthogonal arrage is tested (is shown in Table 2, table
3)。
The oral liquid of table 2 prepares L9(34) orthogonal experiments
The oral liquid of table 3 prepares the results of analysis of variance
Note：F0.01 (2,2)=99；F0.05 (2,2)=19.
From above-mentioned experimental result record sheet 2, table 3, in the range analysis to Orthogonal experiment results, Rj is bigger, right
Experimental result influences bigger.Pass through the range analysis to the experiment：RD>RB>RA>RC is solubilizer>Preservative>Fining agent
>Flavouring.Compare the average index of each factor varying level, preferably, factor D K values are most for the level corresponding to the big person of corresponding K values
That big is K3, and factor B K values maximum is K2, and factor A K values maximum is K1, and factor C K values maximum is that K1 can
Determine that optimised process prepared by oral liquid is：A1B2C1D3, you can to select fining agent as 0.6ml, preservative 0.04g, rectify
Taste agent is 0.02g, solubilizer 0.15ml, blue or green money willow flavones 0.235g, blue or green money willow polysaccharide 1.54g, maniod ebish flower extract 1.9g,
For the best conditions of preparation pr ocess.
1.3.5 stability test
Three parallel control groups of every group of setting, are respectively placed in the environment of normal temperature, high temperature, high humidity in nine groups of experiments of the above,
Investigate its stability.
1. hot test method
The nine groups of oral liquids prepared as stated above, which are placed in 80 DEG C of drying box, to be observed, and its content of dispersion is surveyed after 30 days.
2. high humidity test method
The potassium nitrate solution of configuration saturation is observed in high humidity device, and its content of dispersion is surveyed after 30 days.
3. long-term stable experiment method
The nine groups of oral liquids prepared as stated above, which are placed under normal temperature, to be observed, and its content of dispersion is surveyed after 30 days.
4. assay：Carried out according to the method under 1.3.3 items.
Content of dispersion (normal temperature) after table 4 is tested in each group
Content of dispersion (high temperature) after table 5 is tested in each group
Content of dispersion (high humidity) after table 6 is tested in each group
Above-mentioned each form is analyzed to understand：
1. in three kinds of fining agents, the clarifying effect of AZTC1+1 natural clarifying agents is best.
Found 2. surveying flavones content and sulfuric acid-phynol method by ultraviolet spectrophotometry and surveying polyoses content, second and third, six,
Eight groups of medicament contg is slightly better than other groups.
3. found by three groups of parallel control experiments, it is more stable under the oral liquid higher temperatures high humidity under normal temperature.
4. at second and third, in six, eight groups, the 8th group of bottom precipitation is minimum, and its stabilizing effect is best.Therefore from stability
Effect is seen, the 8th group of optimum formula as the hypoglycemic oral liquid of blue or green money willow Sunset Abelmoschus Root can be selected.8th group of ZTC1+1 is natural
The dosage of fining agent is 0.8ml/10ml, and the dosage of glycerine is 0.25ml/10ml, and the dosage of sodium benzoate is 0.04g/10ml,
The dosage of honey element is 0.025g/10ml.
Embodiment three
Oral liquid hypoglycemic effect research of the present invention.
1.1 test specimen
Qingqian Willow leaf (place of production Xiushui County, jiangxi Province)
Sunset abelmoschus flower
1.2 laboratory apparatus
AUW-220D types electronic balance (Japanese Shimadzu Corporation)
KS-600D Medical ultrasonic cleaners (Ningbo Hai Shu Ke Sheng ultrasonic devices Co., Ltd)
N-1100 Rotary Evaporators (Shanghai Ai Lang Instrument Ltd)
Embedding machine；Microscope (German bresser)
RM-2235 type biological tissue sections machine (German Leica)
1.3 reagent
Alloxan (Sigma companies)；Diabetes pill (Guangzhou Zhongyi Medicine Industry Co., Ltd)；
Blood sugar kit (Maike Tech Co., Ltd., Sichuan Prov.)；Formaldehyde；Physiological saline；
1.4 experimental animal
Healthy SD mouse (cleaning grade), male and female half and half, body weight (20g-30g).
The hypoglycemic experiment of 1.5 mouse
1.5.1 the foundation and packet of diabetic mouse model
Mouse 120 is taken, male and female half and half, 10 is randomly selected and is only used as blank control group (NC), the high sugar of remaining mouse feeding
The feed of high fat one week, then the alloxan solution 65mg/kg of the fresh configuration of tail vein injections, use blood glucose reagent after the 3rd day
Box surveys its fasting blood-glucose to fasting 12h mouse, chooses mouse of the blood glucose higher than 11mmol/l as experimental subjects, randomly selects
Qualified mouse is divided into 11 groups, if diabetic model group (DMC), diabetes pill control group (XKP), and blue or green money willow polysaccharide high dose group
(CPPH), blue or green money willow polysaccharide middle dose group (CPPM), blue or green money willow polysaccharide low dose group (CPPL), blue or green money willow flavones high dose group
(CPFH), blue or green money willow flavones middle dose group (CPFM), blue or green money willow flavones low dose group (CPFL), oral liquid (blue or green money willow polysaccharide+green grass or young crops
Money willow flavones+maniod ebish flower extract) high dose group (PFHH), oral liquid (blue or green money willow polysaccharide+blue or green money willow flavones+sunset abelmoschus flower
Extract) middle dose group (PFHM), oral liquid (blue or green money willow polysaccharide+blue or green money willow flavones+maniod ebish flower extract) low dose group
(PFHL)。
1.5.2 hypoglycemic experiment
Blank control group and the isometric physiological saline of model group gavage, diabetes pill group gavage diabetes pill 40mg/kg are thick more
Sugar is high, normal, basic to give 50mg/kg.d, 25mg/kg.d, 12.5mg/kg.d respectively.General flavone is high, normal, basic to give 9mg/kg.d respectively,
4.5mg/kg.d, 2.25mg/kg.d.Maniod ebish flower extract is high, normal, basic to give 80mg/kg.d, 40mg/kg.d, 20mg/ respectively
kg.d.Oral liquid (blue or green money willow polysaccharide+blue or green money willow flavones+maniod ebish flower extract) senior middle school's low dosage gavage.Continuous gavage 6 weeks,
Fasting blood sugar is surveyed respectively at the 2nd week, the 4th week, the 6th week.
1.5.3 statistical method
Indices withRepresent, the significant difference t methods of inspection between mean
1.5.4 mice pancreatic cellular morphology is observed
The mouse after blood will be taken to take off neck execution, solution takes pancreatic tissue and is immersed in 4% formalin 48 hours, then uses
The ethanol dehydration of more gradients, waxdip, embed, cut into slices, dyeing, mounting, micro- Microscopic observation pancreatic tissue cells form, take pictures,
Record.
1.6 oral liquid hypoglycemic effects are analyzed
1.6.1 influence of the oral liquid (blue or green money willow polysaccharide+blue or green money willow flavones+maniod ebish flower extract) to mouse blood sugar
The blue or green money willow active component of table 7 influences on mouse blood sugar
Note：* p is represented<0.05 has significant difference with model group；* represents P<0.01 has larger significant difference；In bracket
Represent mouse amount.
As can be seen from Table 7 there is blood glucose with blank control group blood glucose without significant changes, model group after naive mice gavage
Significant difference (P<0.01), illustrate that model is successfully established, high, normal, basic group of blue or green money willow polysaccharide and model group blood glucose there were significant differences (P<
0.05), high, normal, basic group of blue or green money willow flavones and model group blood glucose there were significant differences (P<0.01), oral liquid (blue or green money willow polysaccharide+blue or green money
Willow flavones+maniod ebish flower extract) high, normal, basic group with model group blood glucose have significant difference (P<0.01), diabetes pill group and model
Group blood glucose there were significant differences (P<0.01)；But diabetes pill group is can be seen that, polysaccharide high dose group, flavones high dose group, oral liquid (green grass or young crops
Money willow polysaccharide+blue or green money willow flavones+maniod ebish flower extract) high dose group mouse death rate is higher.
1.6.2 the observation of pancreatic tissue cells
Under the microscope：Fig. 3 Normal groups pancreas islet is the cell mass of ellipse, and nucleus is uniform in size, is scattered in pancreas
Between gland acinus, cell quantity is more in pancreas islet, and cell distribution is uniform, and arranged regular is clear in structure, and endochylema enriches, and core circle occupies
In；Fig. 5 is that cell quantity significantly reduces in model group pancreas islet, and cell arrangement is disorderly, and structure is destroyed, and pancreas islet profile disappears, border
It is smudgy；The Pancreas Islet Structure of Fig. 6 diabetes pill groups is more visible, and edge is more neat, but islet cells is distributed sparse, negligible amounts,
Density is relatively low；Fig. 4 oral liquids (blue or green money willow polysaccharide+blue or green money willow flavones+maniod ebish flower extract) middle dose group islet cell mass
More, Pancreas Islet Structure is complete, and islet cells arrangement is more neat, and core circle, endochylema enrich.
At present, treatment diabetes rely primarily on OHA and insulin injection.Wherein, although Western medicine markedly fast, make
With direct, but often there are the adverse reactions such as hypoglycemia and gastrointestinal discomfort.And treatment by Chinese herbs has curative effect stabilization, side effect
It is small, the characteristics of Mutiple Targets act on simultaneously, the treatment of suitable diabetes and its complication.At present for the research at effective active position
Generally screened using Animal Model and cellular level model.
The present invention is optionally to destroy beta Cell of islet by alloxan to cause the function of β cells secrete insulins to send out
Raw obstacle, induces mouse hyperglycaemia, is the low type zoic model with hyperglycemia of insulin, mouse stomach blue or green money willow senior middle school low dosage is more
After six weeks, blood glucose is decreased obviously, and indicates blue or green money willow polysaccharide and flavones is respectively provided with the effect of hypoglycemic, be for sugar and flavones
The hypoglycemic effective active part of blue or green money willow, but when the polysaccharide and flavones of gavage high dose, mouse death rate is larger, Ke Nengyou
There is hypotoxicity effect in the polysaccharide and flavones of high dose, and oral liquid (blue or green money willow polysaccharide+blue or green money willow flavones is understood by embodiment
+ maniod ebish flower extract) middle dosage gavage hypoglycemic effect is most obvious, and mouse death rate is relatively low；From islet cells form point
The islet cells of analysis, polysaccharide and flavones middle dosage is normal, illustrates the joint of blue or green money willow polysaccharide and flavones and maniod ebish flower extract
Using can substantially mitigate and repair damage of the alloxan to Mice Islet Cells, there is the work for improving islet cells morphosis
With.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modification, equivalent substitution or improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (6)
- A kind of 1. hypoglycemic oral liquid, it is characterised in that the raw material comprising following weight ratio：Blue or green money willow polysaccharide 15~30%, it is blue or green Money willow chromocor extract 2~4%, maniod ebish flower extract 15~40%, ZTC1+1 natural clarifying agents 4~6%, sodium benzoate 0.4~0.6%, honey element 0.1~0.2%, glycerine 0.8~1.5%, remaining is water, and raw material summation is 100%.
- 2. a kind of hypoglycemic oral liquid as claimed in claim 1, it is characterised in that each material rate in 10ml oral liquids according to containing There are blue or green money willow polysaccharide 1.54g, blue or green money willow chromocor extract 0.235g, maniod ebish flower extract 1.9g, ZTC1+1 natural clarifying agent 0.6ml, sodium benzoate 0.04g, honey element 0.02g, glycerine 0.15ml, surplus are water.
- 3. a kind of preparation method of hypoglycemic oral liquid as claimed in claim 1 or 2, it is characterised in that by blue or green money willow polysaccharide, green grass or young crops Money willow chromocor extract, maniod ebish flower extract, ZTC1+1 natural clarifying agents, sodium benzoate, honey element, G ＆ W mixing, Through 200 mesh sieve net filtrations, after filling, capping, using 100~120 DEG C of 10~30min of sterilization, room temperature, labeling, outsourcing are cooled to Fill to obtain product.
- A kind of 4. preparation method of hypoglycemic oral liquid as claimed in claim 3, it is characterised in that the blue or green money willow extracting flavonoids Thing and blue or green money willow polysaccharide are made by following steps respectively：1) take blue or green money willow dried leaf to crush, add water to cook three times, merging filtrate, filtering, concentration, after cooling plus absolute ethyl alcohol is to containing Alcohol amount is placed 24 hours, filtering, filtrate is standby respectively with precipitation up to 65%；2) after macroporous absorbent resin pretreatment, upper macroporous absorbent resin after the rotated evaporimeter concentration of filtrate that step 1) is obtained Post, after adsorbing 5 hours, macroreticular resin is rushed with water, 60% ethanol, 85% ethanol, 95% ethanol respectively, collects eluent, thin layer Merge after chromatogram point plate, concentrated with Rotary Evaporators, dried after reclaiming ethanol, produce blue or green money willow chromocor extract；3) precipitation that step 1) obtains is concentrated with Rotary Evaporators, reclaims ethanol, the chlorine of its volume 1/5 is added into concentrate The imitative n-butanol with 1/5,30min is shaken, the mixed liquor after concussion centrifuges 10min under 2000r/min rotating speed, takes out supernatant Liquid, repeats above step 5 times, removes organic solvent portion and protein portion, obtains refined blue or green money willow polysaccharide.
- A kind of 5. preparation method of hypoglycemic oral liquid as claimed in claim 3, it is characterised in that the maniod ebish flower extract Adopt and be prepared by the following steps：Sunset abelmoschus flower crushes, and adds ethanol to decoct three times, merging filtrate, is concentrated after filtering and produce sunset abelmoschus flower Extract.
- A kind of 6. preparation method of hypoglycemic oral liquid as claimed in claim 3, it is characterised in that the ZTC1+1 natural clears Agent, which is adopted, to be prepared by the following steps：Component A and B component are each configured to 1% viscose, first plus B after plus A, stand 6-12 hours be .
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| CN101744850A (en) * | 2008-12-12 | 2010-06-23 | 凌沛学 | Preparation and application of total flavone extracted from plants, as well as pharmaceutical preparations thereof |
| CN105168336A (en) * | 2015-10-08 | 2015-12-23 | 南京轶萃康健康科技有限公司 | Natural medicine composition for adjusting diabetes immune and metabolism functions and preparation method of natural medicine composition |
| CN106509254A (en) * | 2016-10-08 | 2017-03-22 | 湖北三峡神农生物科技有限公司 | Cyclocarya paliurus leaf health-care tea, tablets and manufacture method thereof |
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| CN101744850A (en) * | 2008-12-12 | 2010-06-23 | 凌沛学 | Preparation and application of total flavone extracted from plants, as well as pharmaceutical preparations thereof |
| CN101570557A (en) * | 2009-06-09 | 2009-11-04 | 中国人民解放军第二军医大学 | Compound in cyclocarya paliurus and application thereof in medicament field |
| CN105168336A (en) * | 2015-10-08 | 2015-12-23 | 南京轶萃康健康科技有限公司 | Natural medicine composition for adjusting diabetes immune and metabolism functions and preparation method of natural medicine composition |
| CN106509254A (en) * | 2016-10-08 | 2017-03-22 | 湖北三峡神农生物科技有限公司 | Cyclocarya paliurus leaf health-care tea, tablets and manufacture method thereof |
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