CN107308201A - Preparation method of radix pseudostellariae palpus particle and products thereof and polysaccharide determination method - Google Patents
Preparation method of radix pseudostellariae palpus particle and products thereof and polysaccharide determination method Download PDFInfo
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Abstract
The present invention relates to preparation method of a kind of radix pseudostellariae palpus particle and products thereof and polysaccharide determination method, the preparation method of radix pseudostellariae palpus particle is concretely comprised the following steps：Take radix pseudostellariae to add water to cook extraction twice, merge decoction liquor；Then gained decoction liquor is filtered, is concentrated under reduced pressure into the concentrate that relative density is 1.2~1.5；The particle that medicinal material half weight is made in sucrose is added, appropriate 95% ethanol regulation viscosity is sprayed into, screening granularity is in the particle of 10 60 mesh, and obtaining radix pseudostellariae must particle.And a kind of method for accurately detecting polysaccharide in this medicine granule for treating containing sucrose is provided, this method is simple, accurate, and the quality for control radix pseudostellariae palpus particle provides a kind of accurate detection method.
Description
Technical field
The invention belongs to the field of Chinese medicines, it is related to preparation method of radix pseudostellariae palpus particle and products thereof, further relates to this crown prince
Polysaccharide determination method in ginseng palpus particle.
Background technology
Radix pseudostellariae, Chinese medicine is pinkwort caryophyllaceous ginseng Pseudostellaria heterophylla (Miq.) Pax
Ex Pax et Hoffm. dried root.Build spleen with QI invigorating, it is promoting production of body fluid and nourishing the lung the effect of, clinically for losing the appetite, disease
Weak, spontaneous perspiration is thirsty afterwards and the symptom such as xeropulmonary cough, determines to be included in by the Ministry of Public Health at present and " can be used for the Chinese medicine of health food
List ".It is also the choosing of the optimal tonic of In Guangdong Province people's Baoshang, therefore its price is high all the way.But because radix pseudostellariae has gas cloudy
The effect of giving young employees remedial-courses in general knowledge and vocational skills, for treat deficiency of QI with disinclination to talk, neurolysis, slightly activity it is more with regard to sweating, complexion is redder, night sweating compared with
Many, the symptom such as vexed, dry mouth and throat, the general daily 10-30g of consumption is heavy dose of at most no more than 60g.Radix pseudostellariae must be stone
The fibrous root of bamboo section plant caryophyllaceous ginseng, it is general collect the ramuscule root left after radix pseudostellariae and part cercus is considered to not act on and
Directly abandoned as discarded object, few part is used when tea-drinking or soup stock, and think that it has no medical value, radix pseudostellariae must
Weight accounts for the 10~15% of radix pseudostellariae yield, if can be developed, this to radix pseudostellariae must the comprehensive utilization of resource have
Meaning of crucial importance.
At present, the measure of polysaccharide is used after water extract-alcohol precipitation, and colorimetric estimation is carried out with sulfuric acid-anthrone or sulfuric acid-phynol.Crown prince
Ginseng palpus particle adds a large amount of sucrose as filler in preparation process, and existing polysaccharide determination method is unable to accurate response
Come from many sugar levels of radix pseudostellariae palpus, it is difficult to accurately control its quality.
The content of the invention
In view of this, it is an object of the invention to provide preparation of a kind of radix pseudostellariae palpus particle and products thereof, one is more provided
Plant polysaccharide determination method in accurate radix pseudostellariae palpus particle.
To reach above-mentioned purpose, the present invention provides following technical scheme：
1. the preparation method of radix pseudostellariae palpus particle, the preparation method is following steps：
(1) take radix pseudostellariae palpus extracting in water twice, merge extract solution；
(2) extract solution obtained by step (1) is filtered, is concentrated under reduced pressure into relative density for 1.2~1.5 concentrates；
(3) particle that medicinal material half weight is made in sucrose is added, 95% ethanol regulation viscosity is sprayed into, makes material into particle
And equipment is not glued, screening granularity is in the particle of 10-60 mesh, and obtaining radix pseudostellariae must particle；
The extracting in water is extracted or the refluxing extraction that adds water to add water to cook.
Further, in step (2), the relative density that is concentrated under reduced pressure into is 1.3 concentrate；
Further, in step (1), the extracting in water is first to add water of 10~15 times equivalent to medicinal material weight twice,
Extracted 2~3 hours at a temperature of 85-95 DEG C, extract solution be collected by filtration, filter residue adds water of 6~10 times equivalent to medicinal material weight again,
Continue to extract 0.5~1.5 hour, extract solution is collected by filtration.
Further, in step (1), the extracting in water is first to add water of 10 times equivalent to medicinal material weight twice, in 90
DEG C extract 2~3 hours, be collected by filtration extract solution, filter residue adds water of 7~8 times equivalent to medicinal material weight again, 90 DEG C are extracted 1 hour,
Extract solution is collected by filtration.
Further, in step (3) sucrose addition to ensure to be made the particle of medicinal material half weight, i.e., every 1 gram of radix pseudostellariae
Must 2 grams of particle radix pseudostellariae containing medicinal material palpus.
2. the radix pseudostellariae prepared as the preparation method described in any of the above must particle.
3. the polysaccharide determination method of radix pseudostellariae palpus particle, it is characterised in that determination step is as follows：
(a) hydrolyzate first is obtained with sucrose enzyme hydrolysis radix pseudostellariae palpus particle, the total reducing sugar in hydrolyzate is determined with Phenol-sulphate acid method
Content；
(b) content of reducing sugar in hydrolyzate is determined with DNS methods again, content of reducing sugar is subtracted with total sugar content again by hydrolysis
Extension rate calculates the polyoses content of the radix pseudostellariae palpus particle.
Further, hydrolysis radix pseudostellariae palpus particle is to add 20ml water to dissolve with every 1g radix pseudostellariaes palpus particle in step (a), then is added
10ml sucrose enzyme solutions are mixed, and in 45 DEG C of water bath with thermostatic control 30min, and keep its mixing state.
Further, the sucrose enzyme concentration is 400U/ml.
Further, Phenol-sulphate acid method described in step (a), which is determined as, takes hydrolyzate 1ml constant volumes in 50ml volumetric flasks,
10000r/min centrifugation 10min, supernatant is used as need testing solution；Need testing solution 100l is taken, 2ml is added water to, plus
Enter mass fraction for 5% phenol solution 1.0ml, shake up, be rapidly added mass fraction for 98% concentrated sulfuric acid 5.0ml, shake up, place
5 minutes, put and 15min is heated in boiling water bath, taking-up is cooled to 18-25 DEG C, light absorption value is determined at 490nm, is added together with 2ml water respectively
Make blank Deng reagent, add equivalent reagent to make to calculate total sugar content in hydrolyzate with reference to curve with dextrose standard sample solution.
Further, DNS methods described in step (b), which is determined as, takes hydrolyzate 1ml constant volume, 10000r/ in 50ml volumetric flasks
Min centrifugation 10min, supernatant is used as need testing solution；Need testing solution 1ml is taken again, is added DNS reagent 2.0ml, is shaken
It is even, put and 5min heated in boiling water bath, taking-up be cooled to 18-25 DEG C, add water to 25ml, 540nm at measure absorption value, respectively with
1ml water adds equivalent reagent to make blank, adds equivalent reagent to make to calculate reduction in hydrolyzate with reference to curve with dextrose standard sample solution
Sugared content.
The beneficial effects of the present invention are：1st, the radix pseudostellariae abandoned as discarded object must be made by preparation and conveniently taken
Radix pseudostellariae must particle, have meaning of crucial importance to the comprehensive utilization of radix pseudostellariae resource；2nd, obtained radix pseudostellariae palpus particle is with sugarcane
Sugar is filler, is water-soluble granular, convenient use；3rd, provide a kind of operating method simple, determine accurately detection and contain sugarcane
Measurement of the polysaccharide content method in the radix pseudostellariae palpus particle of sugar, the quality for control radix pseudostellariae palpus particle provides one kind accurately
Detection method.
Embodiment
The preferred embodiments of the present invention are described in detail below.The experiment side of unreceipted actual conditions in embodiment
Method, generally according to normal condition or according to the condition proposed by manufacturer.
The preparation of the radix pseudostellariae of embodiment 1 palpus particle
Claim radix pseudostellariae palpus 100g, be fitted into 3L flasks, add water 1L, soak 30min；Reflux condensing tube is loaded onto on flask, electricity
Hot jacket is heated, and adjusts temperature, keeps micro-boiling 2h；Filtration, collects filtrate, and residue adds water 1L, and heating keeps micro-boiling 1h；Filtration, with
First time filtrate merges；It is 1.2 that filtrate decompression is concentrated into density at -0.075MPa, 75 DEG C, adds sucrose fine 34.1g, is mixed
It is even, spray a small amount of 95% ethanol and adjust sticky, enable material agglomerating, but sieve is not glued, cross No. 2 sieve series and obtain radix pseudostellariae palpus particle
Agent 49.6g.Micro-boiling is between 85-95 DEG C；The amount of sucrose is added to ensure to be made the particle of crude drug half weight, i.e., every 1 gram too
Son ginseng palpus particle radix pseudostellariae containing crude drug must be 2 grams, and following sucrose addition is same.
The preparation of the radix pseudostellariae of embodiment 2 palpus particle
Claim radix pseudostellariae palpus 1000g, be fitted into 20L stainless-steel pan extractors, add water 15L, soak 30min；Adjusting temperature is
95 DEG C, refluxing extraction 2.5h；After cooling, filtrate is collected in filtration, and residue adds water 8L, then refluxing extraction 1.5h, and filter is collected in filtration
Liquid；Merge secondary filtrate, it is 1.3 to be concentrated under reduced pressure into relative density, adds sucrose fine 337g, is mixed, and adjusts moisture, spray into suitable
95% ethanol regulation viscosity is measured, enables material granulating, but does not glue sieve, No. 2 sieve series grains are crossed, obtaining radix pseudostellariae must particle 506g.
The preparation of the radix pseudostellariae of embodiment 3 palpus particle
Claim radix pseudostellariae palpus 500g, be fitted into 20L stainless-steel pan extractors, add water 7.5L, soak 30min；Adjusting temperature is
90 DEG C, refluxing extraction 3h；After cooling, filtrate is collected in filtration, and residue adds water 9L, then refluxing extraction 1.5h, and filtrate is collected in filtration；
Merge secondary filtrate, it is 1.5 to be concentrated under reduced pressure into relative density, adds sucrose fine 165g, is mixed, and adjusts moisture, sprays into 95%
Ethanol in proper amount regulation viscosity, crosses No. 2 sieve series grains, and obtaining radix pseudostellariae must particle 251g.
The preparation of the radix pseudostellariae of embodiment 4 palpus particle
Claim radix pseudostellariae palpus 100g, be fitted into 3L flasks, add water 1.2L, soak 60min；Reflux condensing tube is loaded onto on flask,
Electric jacket is heated, and adjusts temperature, keeps 85-95 DEG C of micro-boiling, 3h；Filtration, collects filtrate, and residue adds water 0.8L, and heating is kept micro-
Boil 1h；Filtration, merges with first time filtrate；It is 1.4 that filtrate decompression, which is concentrated into relative density, adds sucrose fine 33.5g, is mixed
It is even, spray a small amount of 95% ethanol and adjust sticky, enable material granulating, but sieve is not glued, cross No. 2 sieve series and obtain radix pseudostellariae palpus particle
50.2g。
The determination of polysaccharide of the radix pseudostellariae of embodiment 5 palpus particle
Glucose control product solution：Precision is weighed to be dried to the glucose control product 50mg of constant weight at 105 DEG C, puts 50ml appearances
In measuring bottle, it is dissolved in water and is diluted to scale, produces every ml 1mg containing glucose reference substance solution.
The preparation of DNS reagents：Weigh 3,5-dinitrosalicylic acid 6.3g, measure 262ml concentration for 2mol/L hydroxides
Sodium, is added in the hydrothermal solution that 500ml contains 182g sodium potassium tartrate tetrahydrates, along with 5g phenol and 5g sodium sulfites, stirs in the lump
Mix to add water after dissolving, cooling and be settled to 1000ml, produce.Store in standby in brown bottle.
Acetate buffer solution (pH4.5)：Sodium acetate 18.0g, acetic acid 9.8ml on the rocks are taken, adds water and is diluted to 1000ml, is adjusted
PH is produced to 4.5.
Sucrose enzyme solutions：Invertase (200U/mg) 20mg is taken, 10ml is diluted to acetate buffer solution, produces 400U/ml's
Sucrose enzyme solutions；
Need testing solution：Radix pseudostellariae palpus particle 0.1g is taken, is placed in centrifuge tube, the dissolving of 2ml water is added, adds 1ml sucrose
Enzyme solutions, are mixed, and (are shaken frequently) in 45 DEG C of water bath with thermostatic control 30min, are taken this solution 1ml constant volumes in 50ml volumetric flasks, in
10000r/min centrifugation 10min, supernatant is used as need testing solution.
Total reducing sugar bioassay standard curve：Precision draws the μ l of reference substance solution 20,40,60,80,100,120, and 10ml tools are put respectively
Fill in test tube, add water makes final volume be 2.0ml according to this, add the phenol solution 1.0ml that mass fraction is 5%, shake up, rapidly
Addition mass fraction is 98% concentrated sulfuric acid 5.0ml, is shaken up, and places 5 minutes, puts and 15min is heated in boiling water bath, takes out cold with flowing water
To room temperature, another precision extract water 2.0ml is subject to corresponding reagent for blank, the measure absorbance 490nm at, using absorbance as
Ordinate, using mass concentration as abscissa, draws standard curve.
Reducing sugar test standard curve：Precision measures glucose control product solution 0.2,0.4,0.6,0.8,1.0ml, respectively
Put in 25ml tool plug test tubes, add water makes final volume be 1.0ml according to this, adds DNS reagent 2.0ml, shakes up, and puts in boiling water bath and adds
Hot 5min, taking-up is cooled to room temperature with flowing water, adds water to 25ml.Another precision extract water 1.0ml, is subject to corresponding reagent for blank,
Trap is determined at 540nm, using absorbance as ordinate, using concentration as abscissa, standard curve is drawn.
The measure of test sample total reducing sugar：Precision draws the μ l of need testing solution 100, puts in 10ml tool plug test tubes, adds water to 2ml,
The preparation method operation of sighting target directrix curve, from " addition phenol solution 1.0ml ", trap being determined in accordance with the law, with corresponding reagent
For blank, the concentration of need testing solution glucose is read from standard curve, calculates, produces.
The measure of test sample reduced sugar：Precision measures need testing solution 1ml, according to the preparation of reducing sugar test standard curve
Method is operated, and from " adding 2ml DNS reagents ", absorbance is determined in accordance with the law, using corresponding reagent as blank, from standard curve
The concentration of need testing solution is read, calculates, draws the content of reducing sugar in sucrose.
According to more than method measure embodiment 1-2 radix pseudostellariaes must particle, according to the preparation method of embodiment 3 in certain pharmaceutical factory
The product of test manufacture, and the result of control sucrose are as shown in table 1.
Determination of polysaccharide result in the radix pseudostellariae of table 1 palpus particle
| Sample | Specification (g/g) | Total reducing sugar % | Reduced sugar % | Polysaccharide % |
| Embodiment 1 | 2 | 84.23 | 68.16 | 16.07 |
| Embodiment 2 | 2 | 88.67 | 73.42 | 15.25 |
| Certain factory's granule | 2 | 86.91 | 73.73 | 13.18 |
| Sucrose | -- | 107.69 | 107.34 | 0.35 |
Note：Specification is grams of the every gram of granule equivalent to radix pseudostellariae palpus.
As seen from the results in Table 1, this detection method, influence very little of the sucrose to testing result, can accurately detect containing
The radix pseudostellariae of sucrose must in particle polysaccharide content, this to radix pseudostellariae must the quality control of particle be an enforceable scheme.
Finally illustrate, preferred embodiment above is merely illustrative of the technical solution of the present invention and unrestricted, although logical
Cross above preferred embodiment the present invention is described in detail, it is to be understood by those skilled in the art that can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (10)
1. the preparation method of radix pseudostellariae palpus particle, it is characterised in that the preparation method is following steps：
(1) take radix pseudostellariae palpus extracting in water twice, merge extract solution；
(2) by extract solution obtained by step (1), filtration is concentrated under reduced pressure into relative density for 1.2~1.5 concentrates；
(3) particle that medicinal material half weight is made in sucrose is added, it is that 95% ethanol adjusts viscosity to spray into volume fraction, makes material
Equipment into particle and is not sticked, particle of the granularity in 10-60 mesh is screened, obtaining radix pseudostellariae must particle；
The extracting in water is extracted or the refluxing extraction that adds water to add water to cook.
2. preparation method according to claim 1, it is characterised in that in step (1), the extracting in water is first to add twice
Enter water of 10~15 times equivalent to medicinal material weight, extracted 2~3 hours at a temperature of 85-95 DEG C, extract solution, filter residue is collected by filtration
Again plus water of 6~10 times equivalent to medicinal material weight, continue to extract 0.5~1.5 hour, extract solution is collected by filtration.
3. preparation method according to claim 2, it is characterised in that in step (1), the extracting in water is first to add twice
Enter water of 10 times equivalent to medicinal material weight, extracted 2~3 hours in 90 DEG C, extract solution is collected by filtration, filter residue adds equivalent to medicinal material again
The water that 7~8 times of weight, 90 DEG C are extracted 1 hour, and extract solution is collected by filtration.
4. preparation method according to claim 1, it is characterised in that sucrose addition is to ensure that medicine is made in step (3)
The particle of material half weight, i.e., every 1 gram of radix pseudostellariae must 2 grams of particle radix pseudostellariae containing medicinal material palpus.
5. the radix pseudostellariae prepared as the preparation method described in claim any one of 1-4 must particle.
6. the polysaccharide determination method of the radix pseudostellariae palpus particle described in claim 5, it is characterised in that determination step is as follows：
(a) hydrolyzate first is obtained with sucrose enzyme hydrolysis radix pseudostellariae palpus particle, the total sugar content in hydrolyzate is determined with Phenol-sulphate acid method；
(b) content of reducing sugar in hydrolyzate is determined with DNS methods again, content of reducing sugar is subtracted with total sugar content and is diluted again by hydrolysis
Multiple calculates the polyoses content of the radix pseudostellariae palpus particle.
7. polysaccharide determination method according to claim 6, it is characterised in that hydrolysis radix pseudostellariae palpus particle is in step (a)
Add 20ml water to dissolve with every 1g radix pseudostellariaes palpus particle, then add 4000U sucrose enzyme solutions to mix, in 45 DEG C of water bath with thermostatic control 30min, and
Keep its mixing state.
8. the polysaccharide determination method according to claim 6 or 7, it is characterised in that the sucrose enzyme concentration is 400U/ml.
9. polysaccharide determination method according to claim 6, it is characterised in that Phenol-sulphate acid method described in step (a) is determined
To take hydrolyzate 1ml constant volumes in 50ml volumetric flasks, 10000r/min centrifugation 10min, supernatant is molten as test sample
Liquid；The μ l of need testing solution 100 are taken, 2ml is added water to, addition mass fraction is 5% phenol solution 1.0ml, shakes up, is rapidly added matter
Amount fraction is 98% concentrated sulfuric acid 5.0ml, is shaken up, and places 5 minutes, puts and 15min is heated in boiling water bath, and taking-up is cooled to 18-25 DEG C,
Light absorption value is determined at 490nm, adds equivalent reagent to make blank with 2ml water respectively, adds equivalent reagent to make with dextrose standard sample solution
Total sugar content in hydrolyzate is calculated with reference to curve.
10. polysaccharide determination method according to claim 6, it is characterised in that DNS methods described in step (b), which is determined as, to be taken
Hydrolyzate 1ml constant volumes in 50ml volumetric flasks, 10000r/min centrifugation 10min, supernatant is used as need testing solution；Again
Need testing solution 1ml is taken, DNS reagent 2.0ml is added, shakes up, put and 5min is heated in boiling water bath, taking-up is cooled to 18-25 DEG C, adds water
To 25ml, absorption value is determined at 540nm, adds equivalent reagent to make blank with 1ml water respectively, is added together with dextrose standard sample solution
Make to calculate content of reducing sugar in hydrolyzate with reference to curve Deng reagent.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114949027A (en) * | 2022-05-27 | 2022-08-30 | 福建贝迪药业有限公司 | Preparation method of radix pseudostellariae fibrous root extract and application of radix pseudostellariae fibrous root extract in immunoregulation |
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| CN101837041A (en) * | 2010-02-02 | 2010-09-22 | 贵州三元太宝实业股份有限公司 | Method for preparing radix pseudostellariae particles and product thereof |
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| CN101837041A (en) * | 2010-02-02 | 2010-09-22 | 贵州三元太宝实业股份有限公司 | Method for preparing radix pseudostellariae particles and product thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114949027A (en) * | 2022-05-27 | 2022-08-30 | 福建贝迪药业有限公司 | Preparation method of radix pseudostellariae fibrous root extract and application of radix pseudostellariae fibrous root extract in immunoregulation |
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Application publication date: 20171103 |