CN106349401A - Method for optimizing parameters of radix angelica sinensis polysaccharide extracting technology based on response surface method - Google Patents
Method for optimizing parameters of radix angelica sinensis polysaccharide extracting technology based on response surface method Download PDFInfo
- Publication number
- CN106349401A CN106349401A CN201610760826.7A CN201610760826A CN106349401A CN 106349401 A CN106349401 A CN 106349401A CN 201610760826 A CN201610760826 A CN 201610760826A CN 106349401 A CN106349401 A CN 106349401A
- Authority
- CN
- China
- Prior art keywords
- polysaccharide
- radix angelicae
- angelicae sinensis
- volume
- angelica sinensis
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Sustainable Development (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for optimizing parameters of a radix angelica sinensis polysaccharide extracting technology based on a response surface method. The method is used for the polysaccharide extracting technology for Min radix angelica sinensis No.3 produced in Gansu, and comprises the steps that medicinal materials are purified, radix angelica sinensis polysaccharide is extracted with a water-extraction and alcohol-precipitation method, and the extracting rate of polysaccharide in the radix angelica sinensis medicine materials is calculated. According to the method, variable parameters for extraction of radix angelica sinensis polysaccharide are determined with the response surface method, three factors having remarkable influences on the yield of radix angelica sinensis polysaccharide are selected, three-factor and five-level response surface analysis experiments are designed based on single-factor experiments, and then the optimal extraction technology conditions of radix angelica sinensis polysaccharide are determined, wherein according to the optimal extraction technology conditions of radix angelica sinensis polysaccharide, the extraction time is 120 min, the liquid and material ratio of the volume of added water to the mass of the radix angelica sinensis medicine materials is 7:1 ml/g, and the mass concentration of ethyl alcohol in filter liquid is 65%; polysaccharide is extracted under the conditions with the steps in the method, and the calculated yield of measured polysaccharide content is 8.54645%; the difference between the calculated yield and a theoretical prediction value is 0.12379%, and it is fully indicated that optimization carried out on the radix angelica sinensis polysaccharide extracting conditions with the response surface method is reliable and practical.
Description
Technical field
The present invention relates to plant component extraction technical field, specifically one kind optimize Radix Angelicae Sinensis polysaccharide based on response phase method
The method of Extraction technique, the extraction process of " Min the returns No. 3 " Radix Angelicae Sinensis polysaccharide producing for Gansu.
Background technology
When being classified as umbelliferae angelica angelica sinensis(oliv.) dry root of diels, acrid in the mouth warm in nature,
Sweet, Return liver, the heart, spleen channel, there is the effects such as replenishing and activating blood, menstruction regulating and pain relieving, loosening bowel to relieve constipation.Contain in volatile oil Rhizoma Ligustici in Radix Angelicae Sinensis
Ester and butylidenephalide, Phenylpropanoid Glycosides class ferulic acid, polysaccharide etc..Wherein Radix Angelicae Sinensis polysaccharide is the primary water-soluble one-tenth of Radix Angelicae Sinensis
Point, through modern pharmacology experimental study find its have enhancing human body immunity power, radioprotective, enrich blood, antioxidation, antiviral, analgesia,
Hemostasis, antitumor etc. act on." Min returns No. 3 " is the Radix Angelicae Sinensis new varieties that application heavy ion irradiation Biology Breeding technology selects, mesh
Front less to its interior quality research.
The ultimate principle of decoction and alcohol sedimentation technique is that using the most of compositions in the plants such as medical material such as alkaloid salt, glycoside, have
Machine acids, aminoacid, polysaccharide etc. be soluble in water and alcohol in characteristic, gone out with water extraction, and its extracting solution concentrated, it is suitable to add
Ethanol or water are repeated several times sedimentation, remove its insoluble matter, finally obtain clear liquid.
Response phase method (response surface methodology, rsm) is EXPERIMENTAL DESIGN, mathematical statisticss and optimum
A kind of integrated application of change technology, is the product that mathematical method is combined with statistical method, many for being subject to interested response
The problem of individual variable impact is modeled and analyzes, and its final purpose is to optimize this response value.With orthogonal design analytic process and all
Even project analysis and control technique compares, and Responds Surface Methodology is more excellent in terms of EXPERIMENTAL DESIGN and results expression.
Content of the invention
The purpose of the present invention is on the basis of experiment of single factor, using Responds Surface Methodology, " Min returns No. 3 " polysaccharide is carried
Taking technique condition is optimized, and the overall merit for " Min returns No. 3 " quality and exploitation provide reference frame.
For achieving the above object, the technical solution used in the present invention is:
A kind of method optimizing Radix Angelicae Sinensis polysaccharide Extraction technique based on response phase method, when being classified as utilizing heavy ion described in this method
The Radix Angelicae Sinensis new varieties " Min returns No. 3 " that irradiated biological breeding technique selects, are Radix Angelicae Sinensis angelica sinensis(oliv.)
The dry root of diels it is characterised in that: it comprises the following steps:
Step one, medical material remove impurity, weigh appropriate Radix Angelicae Sinensis pulverizing medicinal materials, weigh 10.0g medicine after the sieve screening being 50 mesh with granularity
Material powder is positioned in the round-bottomed flask that capacity is 250ml, adds 80ml petroleum ether to be heated to reflux 1h in 75 DEG C of water-baths, takes out
Filter, discards filtrate, by residue collection to volume for, in the round-bottomed flask of 250ml, adding the ethanol solution that mass concentration is 85%
60ml, flow back 2h, and sucking filtration abandons filtrate, collects filtering residue, in Radix Angelicae Sinensis medical material, oil-soluble impuritieses are removed；
Step 2, decoction and alcohol sedimentation technique extract Radix Angelicae Sinensis polysaccharide, determine the variable parameter that Radix Angelicae Sinensis polysaccharide extracts, setting using response phase method
The test method of three factor five level carries out repeating test acquisition experimental result, calculates Radix Angelicae Sinensis polysaccharide yield, then adopts
Design expert 7.0.0 software carries out multiple regression analysis, show that the regression equation that experimental factor affects on response value is:
In above formula, response value y is the extraction ratio of Radix Angelicae Sinensis polysaccharide, variable parameter x1For alcohol deposition method extraction time, variable parameter x2For institute
Add the volume of water and the liquid ratio of quality of Radix Angelicae Sinensis medical material, variable parameter x3Quality for adding ethanol in filtrate after ethanol is dense
Degree, finally determines x1For 2h, x2For 7ml/g, x3For 66%；
According to described variable parameter, 200ml distilled water in the filtering residue prepared by step one, is added to heat in 80 DEG C of water-baths
Reflux, extract, 2 times, each extraction time is 1h, obtains filtrate, adds the ethanol that mass concentration is 80%, measurement filter in filtrate
After the mass concentration of ethanol reaches 66% postprecipitation 12-24 hour in liquid, filter supernatant, after filtering residue is centrifuged,
Water is added to be dissolved in filtering residue, the volume of added water is 7ml/g with the mass ratio of Radix Angelicae Sinensis medical material, adds chlorine in the solution
The imitative mixed liquor with n-butyl alcohol removes the albumen in solution, obtains Angelica sinensis polysaccharide；
Step 3, by the Angelica sinensis polysaccharide distilled water obtained by step 2 be settled in 100ml volumetric flask be obtained crude polysaccharides molten
Liquid, then take 1.6ml crude polysaccharides solution constant volume in 100ml volumetric flask, the method as standard curve surveys absorbance, calculates and works as
Return the extraction ratio of polysaccharide in medical material.
The computing formula of wherein polysaccharide yield is:
Polysaccharide yield (%)=(crude polysaccharides quality/quality of medicinal material) × 100
Preferably, in described step 2, chloroform and the volume ratio of chloroform in the mixed liquor of n-butyl alcohol and n-butyl alcohol are 4:1.
Preferably, when in described step 2, filtering residue is centrifuged, the rotating speed of centrifuge turns/min for 4000-5000.
Preferably, the formulation of described determination of polysaccharide standard curve, comprises the following steps:
(1) weigh the dilute sulfuric acid constant volume that 100.00mg anthrone mass percent concentration is 76% to volume be in 100ml volumetric flask
Standby；
(2) weigh 105 DEG C of dryings to the glucose 50.00mg of constant mass, plus distilled water constant volume in volume the capacity for 50ml
In bottle, it is made into the Standard glucose solution that mass-volume concentration is 1mg/ml standby；
(3) draw respectively Standard glucose solution 1.0,2.0,3.0,4.0,5.0,6.0ml be placed in the volumetric flask that volume is 50ml
In, plus distilled water constant volume shakes up, then draw the glucose solution 1ml of variant mass concentration respectively, all add the 5ml preparing
Anthrone test solution, is immediately placed in after shaking up in ice-water bath, puts and boils 12min in boiling water bath, and taking-up water rinses 2.5min cooling, standing
It is positioned over mensuration absorbance at wavelength 624nm after 10min, blank is made with distilled water 1.0ml；
(4) with glucose quality concentration be abscissa x, absorbance do regression treatment for vertical coordinate y, obtain regression equation y=
8.2286x-0.0133, r2=0.9983, the range of linearity 20～120 μ g/ml, are depicted as determination of polysaccharide standard curve.
The invention has the benefit that
The present invention determines, using response phase method, the variable parameter that Radix Angelicae Sinensis polysaccharide extracts, and chooses to Radix Angelicae Sinensis polysaccharide yield more significant shadow again
Three factors rung, i.e. the liquid ratio of the quality of alcohol deposition method extraction time, the volume of added water and Radix Angelicae Sinensis medical material, second in filtrate
The mass concentration of alcohol, on the basis of experiment of single factor, design three factor five level response surface analysis experiment, and then determine work as
Return the optimal extract process of polysaccharide.
Brief description
Fig. 1 is the mass concentration of ethanol and polysaccharide yield relation schematic diagram in different filtrates；
Fig. 2 is the different volumes of added water and the liquid ratio of Radix Angelicae Sinensis quality of medicinal material and polysaccharide yield relation schematic diagram；
Fig. 3 is different extraction times and polysaccharide yield relation schematic diagram；
Fig. 4 is the liquid ratio of the volume of extraction time and added water and the quality of Radix Angelicae Sinensis medical material on interacting that polysaccharide yield affects
The schematic diagram of effect；
Fig. 5 is the mass concentration interactive schematic diagram that polysaccharide yield is affected of ethanol in extraction time and filtrate；
Fig. 6 is that the volume of added water is obtained to polysaccharide with the mass concentration of ethanol in the liquid ratio of the quality of Radix Angelicae Sinensis medical material and filtrate
The interactive schematic diagram of rate impact.
Specific embodiment
The present invention is further detailed explanation below in conjunction with the accompanying drawings.
A kind of method optimizing Radix Angelicae Sinensis polysaccharide Extraction technique based on response phase method, when being classified as using weight described in this method
The Radix Angelicae Sinensis new varieties " Min returns No. 3 " that ion irradiation Biology Breeding technology selects, are Radix Angelicae Sinensis angelica sinensis
(oliv.) diels dry root it is characterised in that: it comprises the following steps:
Step one, medical material remove impurity, weigh appropriate Radix Angelicae Sinensis pulverizing medicinal materials, weigh 10.0g medicine after the sieve screening being 50 mesh with granularity
Material powder is positioned in the round-bottomed flask that capacity is 250ml, adds 80ml petroleum ether to be heated to reflux 1h in 75 DEG C of water-baths, takes out
Filter, discards filtrate, by residue collection to volume for, in the round-bottomed flask of 250ml, adding the ethanol solution that mass concentration is 85%
60ml, flow back 2h, and sucking filtration abandons filtrate, collects filtering residue, in Radix Angelicae Sinensis medical material, oil-soluble impuritieses are removed；
Step 2, decoction and alcohol sedimentation technique extract Radix Angelicae Sinensis polysaccharide, determine the variable parameter that Radix Angelicae Sinensis polysaccharide extracts, setting using response phase method
The test method of three factor five level carries out repeating test acquisition experimental result, calculates Radix Angelicae Sinensis polysaccharide yield, then adopts
Design expert 7.0.0 software carries out multiple regression analysis, show that the regression equation that experimental factor affects on response value is:
In formula, response value y is the extraction ratio of Radix Angelicae Sinensis polysaccharide, variable parameter x1For alcohol deposition method extraction time, variable parameter x2For added
Enter the volume of water and the liquid ratio of quality of Radix Angelicae Sinensis medical material, variable parameter x3Quality for adding ethanol in filtrate after ethanol is dense
Degree, finally determines x1For 2h, x2For 7ml/g, x3For 66%；
According to described variable parameter, 200ml distilled water in the filtering residue prepared by step one, is added to heat in 80 DEG C of water-baths
Reflux, extract, 2 times, each extraction time is 1h, obtains filtrate, adds the ethanol that mass concentration is 80%, measurement filter in filtrate
After the mass concentration of ethanol reaches 66% postprecipitation 12-24 hour in liquid, filter supernatant, after filtering residue is centrifuged,
Water is added to be dissolved in filtering residue, the volume of added water is 7ml/g with the mass ratio of Radix Angelicae Sinensis medical material, adds chlorine in the solution
The imitative mixed liquor with n-butyl alcohol removes the albumen in solution, obtains Angelica sinensis polysaccharide；
Step 3, by the Angelica sinensis polysaccharide distilled water obtained by step 2 be settled in 100ml volumetric flask be obtained crude polysaccharides molten
Liquid, then take 1.6ml crude polysaccharides solution constant volume in 100ml volumetric flask, the method as standard curve surveys absorbance, calculates and works as
Return the extraction ratio of polysaccharide in medical material.
In rapid two, chloroform and the volume ratio of chloroform in the mixed liquor of n-butyl alcohol and n-butyl alcohol are 4:1.
When in step 2, filtering residue is centrifuged, the rotating speed of centrifuge turns/min for 4000-5000.
The formulation of determination of polysaccharide standard curve, comprises the following steps:
(1) weigh the dilute sulfuric acid constant volume that 100.00mg anthrone mass percent concentration is 76% to volume be in 100ml volumetric flask
Standby；
(2) weigh 105 DEG C of dryings to the glucose 50.00mg of constant mass, plus distilled water constant volume in volume the capacity for 50ml
In bottle, it is made into the Standard glucose solution that mass-volume concentration is 1mg/ml standby；
(3) draw respectively Standard glucose solution 1.0,2.0,3.0,4.0,5.0,6.0ml be placed in the volumetric flask that volume is 50ml
In, plus distilled water constant volume shakes up, then draw the glucose solution 1ml of variant mass concentration respectively, all add the 5ml preparing
Anthrone test solution, is immediately placed in after shaking up in ice-water bath, puts and boils 12min in boiling water bath, and taking-up water rinses 2.5min cooling, standing
It is positioned over mensuration absorbance at wavelength 624nm after 10min, blank is made with distilled water 1.0ml；
(4) with glucose quality concentration be abscissa x, absorbance do regression treatment for vertical coordinate y, obtain regression equation y=
8.2286x-0.0133, r2=0.9983, the range of linearity 20～120 μ g/ml, are depicted as determination of polysaccharide standard curve.
The variable parameter that Radix Angelicae Sinensis polysaccharide extracts is determined using response phase method, respectively with different alcohol deposition method extraction time (60,
90th, 120,150,180min), the liquid ratio of the quality of the volume of added water and Radix Angelicae Sinensis medical material (6:1,7:1,8:1,9:1,10:
1ml/g), in filtrate, the mass concentration (65%, 70%, 75%, 80%, 85%) of ethanol is that each setting of single factor test 3 repeats to test, and presses
Extract Radix Angelicae Sinensis polysaccharide, Radix Angelicae Sinensis polysaccharide yield when calculating different variable parameter respectively according to the decoction and alcohol sedimentation technique described in step 2.
According to central composite design principle, comprehensive single factor experiment result, choosing has more significant shadow to Radix Angelicae Sinensis polysaccharide yield
3 factors rung, that is, the liquid ratio of the quality of extraction time, the volume of added water and Radix Angelicae Sinensis medical material, in filtrate ethanol matter
Amount concentration, on the basis of single factor experiment, the response surface analysis of design three factor five level is tested, and factor and level are shown in Table 1.
Table 1
First, experiment of single factor result:
(1) impact to " Min returns No. 3 " polysaccharide yield for the mass concentration of ethanol in different filtrates:
Accurately weigh medicinal powder 10.0g, the volume of fixing added water is 6:1ml/ with the liquid ratio of the quality of Radix Angelicae Sinensis medical material
G, extraction time is 60min, and in filtrate, the mass concentration of ethanol is respectively 65%, 70%, 75%, 80%, 85%, according to the method described above
Described step extracts Radix Angelicae Sinensis polysaccharide, and calculates its yield, and result is as shown in Figure 1.
Fig. 1 shows, during precipitate polysaccharides, with the change of the mass concentration of ethanol in filtrate, its polysaccharide yield also has substantially
Change.When the mass concentration of ethanol in filtrate is 70%, polysaccharide yield reaches maximum, and the higher rear polysaccharide yield of concentration drops on the contrary
Low, when being because that the mass concentration of ethanol in filtrate is too high, its impurity also can increase.Therefore by the quality of ethanol in optimal filtrate
Concentration is set to 70%.
(2) volume of different added water and the liquid ratio of the quality of the Radix Angelicae Sinensis medical material shadow to " Min returns No. 3 " polysaccharide yield
Ring:
Accurately weigh medicinal powder 10.0g, the fixed extraction time is 60min, and in filtrate, the mass concentration of ethanol is respectively 70%,
The volume of added water is 6:1,7:1,8:1,9:1,10:1ml/g with the liquid ratio of the quality of Radix Angelicae Sinensis medical material, according to the method described above
Described step extracts Radix Angelicae Sinensis polysaccharide, and calculates its yield, and result is as shown in Figure 2.
Fig. 2 shows, with the increase of amount of water, polysaccharide yield is gradually increased, and when liquid ratio is for 7:1ml/g, polysaccharide obtains
Rate reaches maximum, and subsequent polysaccharide yield is gradually lowered, the liquid of the quality of the therefore optimal volume of added water and Radix Angelicae Sinensis medical material
Material ratio is 7:1ml/g.
(3) the different impacts to " Min returns No. 3 " polysaccharide yield for the extraction time:
Accurately weigh medicinal powder 10.0g, the volume of fixing added water is 7:1ml/ with the liquid ratio of the quality of Radix Angelicae Sinensis medical material
G, in filtrate, the mass concentration of ethanol is respectively 70%, different extraction times is respectively 60,90,120,150,180min, according to
Step described in said method extracts Radix Angelicae Sinensis polysaccharide, and calculates its yield, and result is as shown in Figure 3.
Fig. 3 shows, with the increase of extraction time, polysaccharide yield is gradually increased, many when extraction time reaching 120min
The yield of sugar reaches maximum, and subsequent polysaccharide yield is gradually lowered, and therefore optimal extraction time is 120min.
2nd, response surface optimization experiment
1st, response surface experimental design and result
Using three factor five level of table 1 setting, according to the orthogonal test recording and checking test data, carry out 20 groups of tests,
Wherein there are factorial tests, have multi-center trial, for estimating test error.The results are shown in Table 2.
Table 2
Test data carries out multiple regression analysis using design expert 7.0.0 software, draws experimental factor to response value
The regression equation of impact is:
In above formula, response value y is the extraction ratio of Radix Angelicae Sinensis polysaccharide, variable parameter x1For alcohol deposition method extraction time, variable parameter x2For institute
Add the volume of water and the liquid ratio of quality of Radix Angelicae Sinensis medical material, variable parameter x3Quality for adding ethanol in filtrate after ethanol is dense
Degree.
In equation, the size of every absolute coefficient reflects the influence degree to response value for each factor.Use
Designexpert7.0.0 software carries out the variance analyses of full model response surface to experimental data, the results are shown in Table 3.
Table 3
Notable (p ＜ 0.05) the * * of note: * is extremely notable (p ＜ 0.01)
X as shown in Table 31x3、x2x3、x1 2、x2 2、x3 2Extremely notable on the impact of " Min returns No. 3 " polysaccharide yield, x1、x2、x1x2To polysaccharide
Yield impact is notable, shows that the impact to polysaccharide yield of each factor and its first order and quadratic term is significant.
2nd, the determination of optimal extract process
Using designexpert7.0.0 software, different two factor of impact " Min returns No. 3 " polysaccharide yield is carried out point
Analysis, draws response surface and contour map, sees Fig. 4-Fig. 6.By response surface and contour map, can intuitively embody different two
The reciprocal action to polysaccharide yield response value for the individual factor, the volume of added water and the quality of Radix Angelicae Sinensis medical material as can be seen from Figure
Liquid ratio is the most notable with the reciprocal action of the mass concentration of ethanol in filtrate, shows as overlapping area minimum.3 factors pair
The impact order of " Min returns No. 3 " polysaccharide yield is x3> x2> x1, that is, in filtrate, the mass concentration impact of ethanol is maximum, is added
The liquid ratio of the volume of water and the quality of Radix Angelicae Sinensis medical material is taken second place, and extraction time is minimum.
3rd, confirmatory experiment
According to the regression model of gained, by design expert7.0.0 software, experiment parameter is optimized further, obtain " Min
Return No. 3 " the middle optimum condition extracting polysaccharide: extraction time 127.09min, the volume of added water and the quality of Radix Angelicae Sinensis medical material
Liquid ratio 7.09:1ml/g, the mass concentration 66.06% of ethanol in filtrate, polysaccharide under this optimum process condition " Min returns No. 3 "
Extraction ratio be 8.67024%, for its actual operation, its condition is changed to extraction time 120min, the volume of added water
With the liquid ratio 7: 1ml/g of the quality of Radix Angelicae Sinensis medical material, the mass concentration 66% of ethanol in filtrate, with this understanding according to above-mentioned side
Step described in method extracts polysaccharide, and measuring polyoses content and calculating yield is 8.54645%.Differ 0.12379% with theoretical expectation values,
Absolutely prove that the optimization that Responds Surface Methodology is carried out to Radix Angelicae Sinensis polysaccharide extraction conditions is reliable, have practicality.
Claims (4)
1. a kind of method that Radix Angelicae Sinensis polysaccharide Extraction technique is optimized based on response phase method, described in this method when be classified as using weight from
The Radix Angelicae Sinensis new varieties " Min returns No. 3 " that sub- irradiated biological breeding technique selects, are Radix Angelicae Sinensis angelica sinensis(oliv.)
The dry root of diels it is characterised in that: it comprises the following steps:
Step one, medical material remove impurity, weigh appropriate Radix Angelicae Sinensis pulverizing medicinal materials, weigh 10.0g medicine after the sieve screening being 50 mesh with granularity
Material powder is positioned in the round-bottomed flask that capacity is 250ml, adds 80ml petroleum ether to be heated to reflux 1h in 75 DEG C of water-baths, takes out
Filter, discards filtrate, by residue collection to volume for, in the round-bottomed flask of 250ml, adding the ethanol solution that mass concentration is 85%
60ml, flow back 2h, and sucking filtration abandons filtrate, collects filtering residue, in Radix Angelicae Sinensis medical material, oil-soluble impuritieses are removed；
Step 2, decoction and alcohol sedimentation technique extract Radix Angelicae Sinensis polysaccharide, determine the variable parameter that Radix Angelicae Sinensis polysaccharide extracts, setting using response phase method
The test method of three factor five level carries out repeating test acquisition experimental result, calculates Radix Angelicae Sinensis polysaccharide yield, then adopts
Design expert 7.0.0 software carries out multiple regression analysis, show that the regression equation that experimental factor affects on response value is:
In formula, response value y is the extraction ratio of Radix Angelicae Sinensis polysaccharide, variable parameter x1For alcohol deposition method extraction time, variable parameter x2For added
Enter the volume of water and the liquid ratio of Radix Angelicae Sinensis quality of medicinal material, variable parameter x3For adding the mass concentration of ethanol in filtrate after ethanol,
Final determination x1For 2h, x2For 7ml/g, x3For 66%；
According to described variable parameter, 200ml distilled water in the filtering residue prepared by step one, is added to heat in 80 DEG C of water-baths
Reflux, extract, 2 times, each extraction time is 1h, obtains filtrate, adds the ethanol that mass concentration is 80%, measurement filter in filtrate
After the mass concentration of ethanol reaches 66% postprecipitation 12-24 hour in liquid, filter supernatant, after filtering residue is centrifuged,
Water is added to be dissolved in filtering residue, the volume of added water is 7ml/g with the mass ratio of Radix Angelicae Sinensis medical material, adds chlorine in the solution
The imitative mixed liquor with n-butyl alcohol removes the albumen in solution, obtains Angelica sinensis polysaccharide；
Step 3, by the Angelica sinensis polysaccharide distilled water obtained by step 2 be settled in 100ml volumetric flask be obtained crude polysaccharides molten
Liquid, then take 1.6ml crude polysaccharides solution constant volume in 100ml volumetric flask, the method as standard curve surveys absorbance, calculates and works as
Return the extraction ratio of polysaccharide in medical material.
2. the method optimizing Radix Angelicae Sinensis polysaccharide Extraction technique based on response phase method according to claim 1, its feature exists
In: in the mixed liquor with n-butyl alcohol for the chloroform in described step 2, chloroform and the volume ratio of n-butyl alcohol are 4:1.
3. the method optimizing Radix Angelicae Sinensis polysaccharide Extraction technique based on response phase method according to claim 1, its feature exists
In: when in described step 2, filtering residue is centrifuged, the rotating speed of centrifuge turns/min for 4000-5000.
4. the method optimizing Radix Angelicae Sinensis polysaccharide Extraction technique based on response phase method according to claim 1, its feature exists
In: the formulation of described determination of polysaccharide standard curve, comprise the following steps:
(1) weigh the dilute sulfuric acid constant volume that 100.00mg anthrone mass percent concentration is 76% to volume be in 100ml volumetric flask
Standby；
(2) weigh 105 DEG C of dryings to the glucose 50.00mg of constant mass, plus distilled water constant volume in volume the capacity for 50ml
In bottle, it is made into the Standard glucose solution that mass-volume concentration is 1mg/ml standby；
(3) draw respectively Standard glucose solution 1.0,2.0,3.0,4.0,5.0,6.0ml be placed in the volumetric flask that volume is 50ml
In, plus distilled water constant volume shakes up, then draw the glucose solution 1ml of variant mass concentration respectively, all add the 5ml preparing
Anthrone test solution, is immediately placed in after shaking up in ice-water bath, puts and boils 12min in boiling water bath, and taking-up water rinses 2.5min cooling, standing
It is positioned over mensuration absorbance at wavelength 624nm after 10min, blank is made with distilled water 1.0ml；
(4) with glucose quality concentration be abscissa x, absorbance do regression treatment for vertical coordinate y, obtain regression equation y=
8.2286x-0.0133, r2=0.9983, the range of linearity 20～120 μ g/ml, are depicted as determination of polysaccharide standard curve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610760826.7A CN106349401A (en) | 2016-08-30 | 2016-08-30 | Method for optimizing parameters of radix angelica sinensis polysaccharide extracting technology based on response surface method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610760826.7A CN106349401A (en) | 2016-08-30 | 2016-08-30 | Method for optimizing parameters of radix angelica sinensis polysaccharide extracting technology based on response surface method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106349401A true CN106349401A (en) | 2017-01-25 |
Family
ID=57857740
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610760826.7A Pending CN106349401A (en) | 2016-08-30 | 2016-08-30 | Method for optimizing parameters of radix angelica sinensis polysaccharide extracting technology based on response surface method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106349401A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108732117A (en) * | 2018-05-29 | 2018-11-02 | 山东省中医药研究院 | A kind of extracting method of the Radix Glehniae saccharide compound optimized using response phase method combination genetic algorithm and Direct search algorithm |
| CN108976309A (en) * | 2018-06-29 | 2018-12-11 | 桂林理工大学 | Polysaccharide extracting process and optimization of orthogonal test in passionflower leaf |
| CN109320625A (en) * | 2018-09-26 | 2019-02-12 | 甘肃中医药大学 | A kind of extracting method and application of Radix Angelicae Sinensis polysaccharide |
| CN110283257A (en) * | 2019-06-28 | 2019-09-27 | 浙江理工大学 | A kind of extracting method of Radix Angelicae Sinensis polysaccharide |
| CN112245460A (en) * | 2020-11-09 | 2021-01-22 | 甘肃农业大学 | Preparation method of water decoction of wine angelica and application of active ingredients of water decoction of wine angelica in preparation of medicine for improving immunity |
| CN112908430A (en) * | 2019-12-03 | 2021-06-04 | 中国科学院大连化学物理研究所 | Experimental method for optimizing normal olefin prepared by high-carbon alcohol dehydration by using response surface method |
| CN114343975A (en) * | 2022-01-12 | 2022-04-15 | 河北卫崭医疗科技有限公司 | Wet wound dressing and its prepn |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1631902A (en) * | 2004-11-18 | 2005-06-29 | 武汉大学 | Angelica polysaccharide and its preparation and use |
| CN101235097A (en) * | 2008-02-29 | 2008-08-06 | 武汉大学 | Method for extracting polysaccharide from angelica and application thereof |
| CN104825516A (en) * | 2013-11-15 | 2015-08-12 | 嘉兴职业技术学院 | Response surface method for extracting Solidago canadensis antioxidant component |
| CN104987428A (en) * | 2015-07-23 | 2015-10-21 | 中国科学院西北高原生物研究所 | Compound enzyme-microwave extraction method for optimizing Nitraria polysaccharide by response surface methodology |
-
2016
- 2016-08-30 CN CN201610760826.7A patent/CN106349401A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1631902A (en) * | 2004-11-18 | 2005-06-29 | 武汉大学 | Angelica polysaccharide and its preparation and use |
| CN101235097A (en) * | 2008-02-29 | 2008-08-06 | 武汉大学 | Method for extracting polysaccharide from angelica and application thereof |
| CN104825516A (en) * | 2013-11-15 | 2015-08-12 | 嘉兴职业技术学院 | Response surface method for extracting Solidago canadensis antioxidant component |
| CN104987428A (en) * | 2015-07-23 | 2015-10-21 | 中国科学院西北高原生物研究所 | Compound enzyme-microwave extraction method for optimizing Nitraria polysaccharide by response surface methodology |
Non-Patent Citations (1)
| Title |
|---|
| 纪鹏 等: "响应面分析法优化当归粗多糖提取工艺", 《天然产物研究与开发》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108732117A (en) * | 2018-05-29 | 2018-11-02 | 山东省中医药研究院 | A kind of extracting method of the Radix Glehniae saccharide compound optimized using response phase method combination genetic algorithm and Direct search algorithm |
| CN108976309A (en) * | 2018-06-29 | 2018-12-11 | 桂林理工大学 | Polysaccharide extracting process and optimization of orthogonal test in passionflower leaf |
| CN109320625A (en) * | 2018-09-26 | 2019-02-12 | 甘肃中医药大学 | A kind of extracting method and application of Radix Angelicae Sinensis polysaccharide |
| CN112870215A (en) * | 2018-09-26 | 2021-06-01 | 甘肃中医药大学 | Application of angelica polysaccharide |
| CN110283257A (en) * | 2019-06-28 | 2019-09-27 | 浙江理工大学 | A kind of extracting method of Radix Angelicae Sinensis polysaccharide |
| CN112908430A (en) * | 2019-12-03 | 2021-06-04 | 中国科学院大连化学物理研究所 | Experimental method for optimizing normal olefin prepared by high-carbon alcohol dehydration by using response surface method |
| CN112245460A (en) * | 2020-11-09 | 2021-01-22 | 甘肃农业大学 | Preparation method of water decoction of wine angelica and application of active ingredients of water decoction of wine angelica in preparation of medicine for improving immunity |
| CN114343975A (en) * | 2022-01-12 | 2022-04-15 | 河北卫崭医疗科技有限公司 | Wet wound dressing and its prepn |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106349401A (en) | Method for optimizing parameters of radix angelica sinensis polysaccharide extracting technology based on response surface method | |
| CN106309521A (en) | Method for optimizing process parameters of angelica sinensis total flavonoid extraction with response surface methodology | |
| CN106018576B (en) | A kind of method for building up of Zaizao Pill UPLC finger-prints | |
| CN102579667B (en) | Preparation method of donkey-hide gelatin and Angelica blood-nourishing particles | |
| CN110527000A (en) | A kind of method that polygonatum cyrtonema aerial part extracts polysaccharide | |
| CN107251728A (en) | A kind of extracting method of dendrobium candidum | |
| CN102422956A (en) | Anti-aging health-care tea | |
| CN107115460A (en) | David's-harp compound granules and preparation method thereof | |
| CN109985097A (en) | A kind of preparation method of Compound Jinyinhua Granules | |
| CN101690757B (en) | Method for preparing bezoar supernatant preparations | |
| CN103479751B (en) | Method for combined extraction of tritepenoidic acid, polyphenols and polysaccharides in loquat flower | |
| CN101897770B (en) | Bone spur capsule and preparation process thereof | |
| CN106317242A (en) | Method for optimizing process parameters of incarvillea sinensis polysaccharide extraction with response surface methodology | |
| CN103301291B (en) | Arillus Longan vigorate qi and replenish the blood soup and preparation method thereof and quality determining method | |
| CN102716255A (en) | Eucommia ulmoides medicinal wine and preparation method thereof | |
| CN102441086A (en) | Guiqi blood-nourishing oral liquid | |
| CN105055497A (en) | Sijunzi decoction tea and preparation process thereof | |
| CN106063828B (en) | A kind of oil extracting method of tree peony blade polyphenol | |
| CN106841470A (en) | The efficient liquid phase characteristic spectrum and its acquisition methods of a kind of dried immature fruit of citron orange processed products of Rhizoma Atractylodis Macrocephalae | |
| CN106540233A (en) | A kind of preparation method of tangerine peel bamboo shavings granule | |
| CN101869644A (en) | Dark-skinned chicken dispersible tablet and preparation process thereof | |
| CN107961321A (en) | A kind of extraction process of six directions pellet bulk pharmaceutical chemicals | |
| CN106699329A (en) | Chrysanthemum indicum polysaccharide-containing foliar fertilizer composition and application thereof | |
| CN104001014A (en) | Unibract fritillary bulb lung-heat-clearing syrup and production process thereof | |
| CN105380997A (en) | Method for preparing ligustrum lucidum ait |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170125 |
|
| RJ01 | Rejection of invention patent application after publication |