CN105817643B - A method of waste prepares nanoparticle after extracting saponin using ginseng - Google Patents
A method of waste prepares nanoparticle after extracting saponin using ginseng Download PDFInfo
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- CN105817643B CN105817643B CN201610295516.2A CN201610295516A CN105817643B CN 105817643 B CN105817643 B CN 105817643B CN 201610295516 A CN201610295516 A CN 201610295516A CN 105817643 B CN105817643 B CN 105817643B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses the methods that waste after a kind of extraction saponin with ginseng prepares nanoparticle.It is the waste after extracting saponin using ginseng, quickly by Ag in a mild condition+、Au3+It is reduced into silver nano-grain and gold nano grain respectively.Key step: cleaning ginseng extracts saponin waste first, and drying removes residual alcohols, collects sieving dry product；The dregs of a decoction after proposing processing with sterile boiling merging filtrate and are centrifuged after filtering；Extracting solution after taking centrifugation is mixed with sterile water, and gold chloride or silver nitrate solution are added into reaction system, reduction reaction occurs in shaking bath at 60-80 DEG C, nanoparticle is collected by centrifugation after reaction.Simple process and low cost of the invention is swift in response, environmental-friendly, and obtained product has dispersibility and stability well, metal nanoparticle colloidal sol easy to form in aqueous solution.Chinese medicine dreg comprehensive utilization of resources added value can be improved in this method.
Description
Technical field
The invention belongs to metal nano material synthetic technologys, more particularly, to discarded after a kind of extraction saponin using ginseng
Object extracting solution is come the method for preparing silver nanoparticle and gold nano grain.
Background technique
The biosynthesis of nano material is a kind of green synthesis method for combining nanotechnology and biotechnology.It compares
The synthesis methods for nanoparticles such as traditional physics and chemistry, the biosynthesis of nano material is in the selection of raw material, reaction condition
The more environmentally-friendly health of regulation and post-processing etc..The common raw material of nano material biological synthesis process has microorganism, enzyme or plant
Object etc..Compared with microorganism and enzyme, Bacteria Culture link can be omitted using induction biosynthesis nano material, preparation process is relatively simple
It is single, it is synthesized more suitable for extensive nanoparticle.
Jilin Province is the world's largest ginseng place of production, and ginseng planting's area is 7200 hectares, and only gen-seng haulms annual output is super
Cross 5000 tons.Contain various bioactive components in gen-seng haulms and ginseng, such as panaxoside, flavonoids and triterpenes
Close object, amino acid, peptide, volatile oil, fatty acid etc..There is the wastings of resources, purity for the traditional extraction technique of ginsenoside
The disadvantages of relatively low, effective component is lost.Pan Huafeng etc. extracts ginseng according to 2005 editions Chinese Pharmacopoeia the methods and extracts soap
Tri- kinds of content of ginsenoside of Rg1, Rb1 and Re are substantially reduced compared with Ginseng extract content in the dregs of a decoction after glucoside, but still are accounted for and always mentioned
20% or more (Traditional Chinese Medicine University Of Guangzhou's journal, 2012,29,428-431) of taken amount shows that there are still a large amount of in the ginseng dregs of a decoction
Active constituent.According to incompletely statistics, only just up to 30,000,000 tons of plant dregs of a decoction annual emissions, dregs of a decoction processing have become in China
Can not be ignored the problem of in Chinese herbal medicine and Chinese patent drug process of manufacture.Chinese medicine dreg resource reutilization new way is opened up,
Its bring environmental pollution and security risk are reduced or eliminated, the only way of Development of Industries of Modem Traditional Chinese Medicine is become.
Plant biomass reduction method is prepared metal nanoparticle and refers mainly to be carried out using plant extracts as reducing agent
Nanoparticle synthesis.Many plants have been reported for nanoparticle synthesis, such as aloe, alfalfa, lemon grass (Cymbopogon citratus), lemongrass, Luo Wang
Cotyledon etc..Patent 200610135256.9,200910112113.X, which are reported, carries out gold, silver and palladium nanometer using plant extraction liquid
The synthesis of particle.Patent 200910110902.X, which is reported, prepares monocrystal silver nano line using sausage leaf extract reduction method.Text
It offers search result and shows to have no that extracting saponin waste as raw material using the dregs of a decoction, especially ginseng prepares metal nanoparticle
Domestic and international relevant report.
Summary of the invention
The present invention is intended to provide a kind of quickly will using the waste extracting solution after ginseng extraction saponin in a mild condition
Ag+、Au3+It is reduced into the method for silver nano-grain and gold nano grain respectively.
Metal nanoparticle preparation method of the present invention is that ginseng extracts the waste pretreatment after saponin first,
It the steps include: that weighing ginseng extracts saponin waste residue 50-100g, is added 300-500ml distilled water, stirs evenly, 10,000-
It is centrifuged 10-15min under 16,000 rpm, the non-ginseng powdered rubber after discarding supernatant liquor and a small amount of layering repeats 1-2
It is secondary；In 50-70 DEG C of drying 12-24h, residual alcohols and moisture in the dregs of a decoction are removed, is collected by being done after 0.425-0.850mm mesh
Product.Metal nanoparticle preparation method of the present invention, followed by prepares plant extraction liquid, the steps include: to take at 10-20g
Dry product after reason is boiled with sterile water 200-300ml and mentions 3 times, first time 2-3h, the 2nd time and the 3rd time 1-2h, is cooled to room temperature filtering,
Merge filtrate after filtering 3 times.10-15min is centrifuged at 10,000-16,000 rpm.Water extract after centrifugation is placed on 4 DEG C of ice
It is spare in case.
Gold nano grain preparation method of the present invention the steps include: the extraction for taking 5ml ginseng to extract saponin waste
Liquid is uniformly mixed with 10ml sterile water first, then to addition 5-15ml chlorauric acid solution in system, at a temperature of 60-80 DEG C
React 15-30min.Concentration of the gold chloride in reaction mixture is 0.001-0.01mol/L.
Silver nano-grain preparation method of the present invention the steps include: to take 5ml ginseng to extract saponin waste extracting solution,
It is uniformly mixed first with 25ml sterile water, then to 10-20ml silver nitrate solution is added in system, at a temperature of 60-80 DEG C instead
1-3h is answered, concentration of the silver nitrate in reaction mixture is 0.001-0.01mol/L.
Nanometer grain preparation method of the present invention the steps include: after reaction, at 10,000-16,000 rpm
It is centrifuged 10-15min, collects nanoparticle, with sterile water wash 2-3 times, 6-8h is then dried at 30-50 DEG C.
Ginseng of the present invention extracts saponin waste reduction method and gold nano grain and silver nano-grain, gained ball is made
The partial size of shape gold nano grain is in 10-20nm, and the partial size of silver nano-grain is in 5-15nm.
Main advantages of the present invention:
Technique letter of the invention is answered, and is swift in response, and the additive in addition to silver nitrate and gold chloride is not needed, obtained
Nanoscale Argent grain and gold particle have dispersibility and stability well, metal nanoparticle easy to form in aqueous solution
Colloidal sol.This method is the new method that a kind of ginseng extracts that waste after saponin recycles, and Chinese medicine dreg comprehensive resource can be improved
Utilize added value.
Detailed description of the invention
Fig. 1 is the Flied emission transmission electron microscope picture for the gold nanoparticle that the present invention is implemented；
Fig. 2 is the Flied emission transmission electron microscope picture for the Nano silver grain that the present invention is implemented.
Specific embodiment
Below by specific example, the invention will be further described.
Embodiment 1
The method for preparing gold nanoparticle using waste after ginseng extraction saponin, it is characterized in that: weighing white ginseng (Jilin people
Ginseng) the waste 100g after saponin is extracted, 500ml distilled water is added, stirs evenly, 15min is centrifuged at 10,000rpm, abandons
Fall supernatant liquor and be layered non-ginseng powdered rubber on a small quantity, is repeated 1 times；It is dried in 60 DEG C of baking ovens for 24 hours, removes and remained in the dregs of a decoction
Alcohols and moisture collect the dry product after sieving by 0.425mm；Continue to promote product three times with the sterile boiling of 500ml, first time 2h,
It second and each 1h of third time, is cooled to room temperature and filters, merge filtrate after filtering three times, be then centrifuged at 15,000rpm
15min removes suspended matter；Extracting solution after taking 5ml to be centrifuged, is uniformly mixed with 10ml sterile water first, then adds 10ml concentration and is
0.005mol/L chlorauric acid solution is reacted and is carried out on 80 DEG C, the shaking bath of 200r/min, the reaction mixture observed
Color gradually becomes purple, shows there is gold nanoparticle generation in reaction.After reacting 30min, it is centrifuged under the conditions of 16,000rpm
15 minutes, gold nanoparticle is collected, with 6h dry at sterile water wash 3 times, 50 DEG C.Uv-vis spectra detects reaction mixing
Object has a highest peak at 540nm, this is the characteristic peak of gold nanoparticle.The aurosol obtained by transmission electron microscope observing, gained gold
Nano particle is spherical shape, and particle diameter distribution is in 10 ~ 20nm(attached drawing 1).
Embodiment 2
The method for preparing Nano silver grain using waste after ginseng extraction saponin, it is characterized in that: taking red ginseng (American Ginseng)
60 grams of waste after extracting saponin, 500ml distilled water is added, stirs evenly, is centrifuged 15min at 10,000rpm, discards
Layer and is layered non-ginseng powdered rubber at clear liquid on a small quantity, is repeated 1 times；It is dried in 60 DEG C of baking ovens for 24 hours, removes residual alcohols in the dregs of a decoction
And moisture, collect the dry product after sieving by 0.425mm.Continue to promote product three times with the sterile boiling of 500ml, first time 2h, second
Secondary and each 1h of third time, is cooled to room temperature and filters, merge filtrate after filtering three times, be then centrifuged 15min at 15,000rpm
Remove suspended matter.Extracting solution after 5ml is centrifuged is weighed, is uniformly mixed first with 10ml sterile water, then adding 15ml concentration is
0.01mol/L silver nitrate solution reacts and carries out on 80 DEG C, the shaking bath of 200r/min, observes reaction mixture face
Color gradually becomes brown, shows there is Nano silver grain generation in reaction.After reacting 3h, it is centrifuged under the conditions of 16,000rpm
15min collects nanoparticle, with sterile water wash 3 times, 50 DEG C of dry 6h.Uv-vis spectra detects that reaction mixture exists
There is a highest peak at 415nm, this is the characteristic peak of Nano silver grain.The silver sol obtained by transmission electron microscope observing, gained silver nanoparticle
Particle is spherical shape, and particle diameter distribution is in 5-15nm(attached drawing 2).
Claims (2)
1. the method for preparing gold nanoparticle using waste after white ginseng extraction saponin, it is characterized in that: weighing white ginseng extracts saponin
Waste 50-100g afterwards is added 300-500ml distilled water, stirs evenly, be centrifuged 10- at 10,000-16,000rpm
15min discards supernatant liquor and is layered non-white ginseng powdered rubber on a small quantity, repeats 1-2 times；12- is dried in 50-70 DEG C of baking oven
For 24 hours, residual alcohols and moisture in the waste after white ginseng extracts saponin are removed, the dry product after sieving by 0 .425mm is collected；It takes
Dry product is promoted product 3 times, the 1st 2-3h, the 2nd time and the 3rd each 1-2h with the sterile boiling of 200-500ml after 10-20g sieving, cold
But to room temperature and filter, merge filtrate after filtering three times, be then centrifuged at 10,000-16,000rpm 10-15min remove it is outstanding
Floating object；Extracting solution after taking 5ml to be centrifuged, is uniformly mixed with 10ml sterile water first, and then adding 5-15ml concentration is 0
.005mol/L chlorauric acid solution is reacted and is carried out on 60-80 DEG C, the shaking bath of 200r/min, reacts 15-30min；16,
It is centrifuged 10-15min under the conditions of 000rpm, collects gold nanoparticle, with drying 6-8h at sterile water wash 2-3 time, 30-50 DEG C,
Gained gold nanoparticle is spherical shape, and particle diameter distribution is in 10-20nm.
2. the method for preparing Nano silver grain using waste after red ginseng extraction saponin, it is characterized in that: after taking red ginseng to extract saponin
50-100 grams of waste, be added 300-500ml distilled water, stir evenly, be centrifuged 10- at 10,000-16,000rpm
15min discards supernatant liquor and is layered non-Red Ginseng substance on a small quantity, repeats 1-2 times；12- is dried in 50-70 DEG C of baking oven
For 24 hours, residual alcohols and moisture in the waste after red ginseng extracts saponin are removed, the dry product after sieving by 0.425mm is collected, takes
Dry product is promoted product 3 times, the 1st 2-3h with the sterile boiling of 200-500ml after 10-20g sieving, and second and each 1-2h of third time,
It is cooled to room temperature and filters, merge filtrate after filtering three times, be then centrifuged 10-15min at 10,000-16,000rpm and remove
Suspended matter；Extracting solution after 5ml is centrifuged is weighed, is uniformly mixed first with 10ml sterile water, then adding 5-15ml concentration is
0.01mol/L silver nitrate solution is reacted and is carried out on 60-80 DEG C, the shaking bath of 200r/min, after reacting 3h, 16,
It is centrifuged 10-15min under the conditions of 000rpm, collects Nano silver grain, with sterile water wash 3 times, 30-50 DEG C of dry 6h, gained is silver-colored
Nanoparticle is spherical shape, and particle diameter distribution is in 5-15nm.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107282940B (en) * | 2017-06-13 | 2021-02-19 | 上海理工大学 | Method for preparing gold nanoparticles by using pseudo-ginseng extracting solution |
| CN107685152A (en) * | 2017-07-03 | 2018-02-13 | 上海理工大学 | A kind of method that silver nano-grain is prepared using Sargent gloryvine extract solution |
| CN107855541A (en) * | 2017-11-30 | 2018-03-30 | 上海理工大学 | A kind of method that silver nano-grain is prepared using pseudo-ginseng leaching liquor |
| CN109128214A (en) * | 2018-09-03 | 2019-01-04 | 黄冈师范学院 | A kind of method that Radix Isatidis residue prepares copper nanoparticle |
| CN110625133B (en) * | 2019-09-11 | 2022-10-21 | 陕西中医药大学 | Method for preparing silver nanoparticles from traditional Chinese medicine residues and application thereof |
| CN113814406A (en) * | 2021-09-17 | 2021-12-21 | 中硕实业(上海)有限公司 | Method for biologically synthesizing silver nanoparticles |
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| CN101498037A (en) * | 2009-01-14 | 2009-08-05 | 厦门大学 | Method for preparing single crystal silver nano-wire by plant biomass reduction |
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| CN102240815A (en) * | 2011-06-16 | 2011-11-16 | 广东工业大学 | Method for preparing nano silver particles by using plant extract for reduction, and application of method |
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Patent Citations (5)
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|---|---|---|---|---|
| CN102202815A (en) * | 2008-05-16 | 2011-09-28 | 维鲁泰克技术股份有限公司 | Green synthesis of nanometals using plant extracts and use thereof |
| CN101498037A (en) * | 2009-01-14 | 2009-08-05 | 厦门大学 | Method for preparing single crystal silver nano-wire by plant biomass reduction |
| CN101912976A (en) * | 2010-08-24 | 2010-12-15 | 厦门大学 | Method for preparing silver nano granules by reducing plant extract |
| CN102240815A (en) * | 2011-06-16 | 2011-11-16 | 广东工业大学 | Method for preparing nano silver particles by using plant extract for reduction, and application of method |
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