CN102240059A - Method for preparing bacteriostat and application of acorn extract used as bacteriostat - Google Patents

Method for preparing bacteriostat and application of acorn extract used as bacteriostat Download PDF

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CN102240059A
CN102240059A CN2011101264376A CN201110126437A CN102240059A CN 102240059 A CN102240059 A CN 102240059A CN 2011101264376 A CN2011101264376 A CN 2011101264376A CN 201110126437 A CN201110126437 A CN 201110126437A CN 102240059 A CN102240059 A CN 102240059A
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acorn
extract
concentrate
bacteriostat
bacteriostatic agent
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CN102240059B (en
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李安平
谢碧霞
丁彦鹏
王森
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Central South University of Forestry and Technology
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Central South University of Forestry and Technology
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Abstract

The invention discloses a method for extracting a bacteriostat and application of an acorn extract used as the bacteriostat. The method comprises the following steps of: washing fresh acorns and removing impurities; drying at the drying temperature of between 40 and 80 DEG C, and grinding to obtain acorn powder; adding into solution of methanol, leaching, and refluxing in water bath to obtain leaching liquor; concentrating the leaching liquor to obtain concentrated solution; and adding the concentrating solution into extract liquor and extracting to remove fat, continuing to concentrate in boiling water bath after degreasing until a concentrate is dry to obtain paste, adding solution of acetone into paste and dissolving, extracting for 2 to 4 times, filtering, mixing filtrate, and concentrating and drying to obtain the acorn extract bacteriostat. The acorn extract prepared by the method has remarkable effects of inhibiting Staphylococcus aureus and Escherichia coli. The bacteriostat can be used for corrosion prevention and bacteriostasis of foods and medicines.

Description

A kind of method for preparing bacteriostatic agent and acorn extract are as the application of bacteriostatic agent
Technical field
The present invention relates to a kind of preparation method of food additives, is a kind of preparation method of bacteriostatic agent specifically, also relates to the application of acorn extract as bacteriostatic agent.
Background technology
Acorn is the general name of Fagaceae vegetable seeds.Study of Acorn Resources in China is abundant, and is various in style, produces acorn 60~7,000,000,000 kg per year.Every acorn mature period is seen everywhere in the central mountain Songshan, and the acorn that comes off naturally causes the significant wastage of resource.At present, acorn is except that being used for weaving, extraction tannin extract and making bean curd on a small quantity, and major part is not utilized effectively.
Anticorrisive agent can be divided into natural antiseptic agent and synthetic preservative two big classes according to the source.Most synthetic preservative is unfavorable to human body, as benzoic acid, just has antimicrobial spectrum narrow, and taste is not good, and edible for a long time or excessive amount is to shortcomings such as health cause damage.Characteristics such as natural antiseptic agent has safety non-toxic, and antibiotic property is good have become focus about the research of natural antiseptic agent.
Natural antiseptic agent is mainly derived from plant, animal and microorganism, wherein derive from the maximum of plant, and antibiotic property is better.The number of applying for a patent a kind of preparation method of Bitter Melon P.E bacteriostatic agent that has been 200810147316.8 patent disclosure, this anticorrisive agent fungistatic effect is better, but cost is higher.The invention provides a kind of is the broad-spectrum antiseptic of raw material with the acorn, low cost, and bacteriostatic agent preparation method simple to operate, and with the application of acorn extract in bacteriostatic agent.
Summary of the invention
The invention provides the application as bacteriostatic agent of a kind of preparation method of bacteriostatic agent and acorn extract, is raw material with the acorn, the products material wide material sources, and extracting method is simple to operate, can reduce cost.
It is raw material that the present invention adopts acorn, and its concrete steps are
(1) fresh acorn is cleaned impurity elimination;
(2) when bake out temperature is 40 ℃-80 ℃, dry, be milled to the acorn powder;
(3) add and to carry out carrying out after the lixiviate water-bath in the methanol solution and reflux and obtain leaching liquor;
(4) after being concentrated, leaching liquor obtains concentrate;
(5) concentrate is added extract in the extract and sloughs fat,
(6) in boiling water bath, continue to be concentrated into the dried paste that obtains after the degreasing,
(7) paste is added the acetone soln dissolving, extract 2-4 time, filter, merging filtrate, concentrate drying promptly get the acorn extract, and this acorn extract is bacteriostatic agent.
Described acorn is the general name of Fagaceae vegetable seeds, comprises chinquapin, Mao Li, little red evergreen chinquapin, cork oak, bitter sweet oak, struggle against lithocarpus glaber, southeast lithocarpus glaber, U.S. leaf lithocarpus glaber, the lithocarpus glaber that comes into leaves, Duo Mai Qinggang, spire Qinggang, Da Ye Qinggang firmly.
Acorn is starch-containing mostly to be 50%~70% greatly, soluble sugar 2%~15%, tannin 0.26%~17.74%, protein 1.17%~8.72%, grease 1.04%~6.86%, crude fibre 1.13%~5.89%, ash content 1.30%~3.40%.Wherein lithocarpus glaber genus and Castanea content of starch are higher, can reach 60%~80%; Tannin content belongs to the highest with oak, most kinds reach more than 10%; Grease is rich with the beech in Quercus acutissima, tobacco pipe lithocarpus glaber, Guilin evergreen chinquapin and the Cyclobalanopsis, bright leaf beech equal size, reaches 14.79%, 17%, 20%, 40%~46% and 49% respectively; Some kind vitamin B2 content is abundant, is higher than 7~10 times in grain, is respectively 54.2,54.2 and 63.3 μ g/g as Cortex Querci franchetii, yellow back of the body Qinggang and Qinggang.In addition, rubber benevolence also contains the materials such as five carbon glycan, vitamin B1, vitamin C, Yan acid, pigment, mineral matter, datiscetin and carbohydrate thereof of some.
Tannin is tannic acid or tannic acid again, is divided into Hydrolysable Tannins (HT) and condensed tannin (CT).That tannin has is anti-oxidant, conjugated protein, anticorrosion, in conjunction with polysaccharide, antibacterial and function such as preserve moisture.Because the acorn raw material sources are extensive, utilization rate is low, and contains great deal of tannin class material, is used to extract bacteriostatic agent to exploitation wild plant Study of Acorn Resources, and the economy that develops forestry provides a new approach.
The degree of grinding of described acorn powder is the 30-100 order.
The concentration of described methanol solution is 40%-80%, during lixiviate and the solid-to-liquid ratio of acorn powder be 1: 3-1: 15.
The temperature that described water-bath refluxes is 70-90 ℃, and return time is 2h-4h.
Described extract is benzinum, ethyl acetate or dichloromethane solution, and wherein the volume ratio of extract and concentrate is 1: 1.
The volume ratio of described acetone soln and dope is 1: 2-1: 10.
Described filtrate method for concentration is that normal pressure or decompression concentrate, and dry is vacuum drying, and baking temperature is 30-50 ℃.
Also relate to of the application of acorn extract as bacteriostatic agent.
The present invention compared with prior art, with acorn as the raw material that extract bacteriostatic agent, its wide material sources, various in style; This bacteriostatic agent preparation method is simple, and used solvent is all recyclable to be utilized again, and easy to operate, cost is low, is easy to suitability for industrialized production; This bacteriostatic agent fungistatic effect is obvious, nontoxic, environmental friendliness; This bacteriostatic agent scope of application is wide, can be widely used in food, the medicine, and effect is obvious, only needs 3/10000ths to five can reach fungistatic effect.
The specific embodiment
Below by this patent of concrete implementation:
Embodiment 1:
Take by weighing the acorn 50g of 40 ℃ of oven dry, add 80% methanol solution 150mL, in the 250mL round-bottomed flask, filter behind 70 ℃ of water-bath backflow 2h, the leaching liquor vacuum is concentrated into 50mL according to 1: 3 solid-to-liquid ratio.Add isopyknic petroleum ether extraction in the concentrate to slough fat.In boiling water bath, continue to be concentrated into dried after the degreasing, obtain sticky paste.With the paste volume ratio is 1: 2 acetone solution, filters, and repeats 2 times, merges collection filtrate.Filtrate decompression is concentrated into 20mL, and vacuum drying under 50 ℃ of conditions promptly gets the bacteriostatic agent finished product.
Embodiment 2:
Take by weighing the acorn 50g of 80 ℃ of oven dry, add 60% methanol solution 250mL according to 1: 5 solid-to-liquid ratio, in the 500mL round-bottomed flask, 85 ℃ of water-bath backflow 3h repeat 2 times, can suitably reduce methanol usage for the second time, merge and filter, the leaching liquor vacuum is concentrated into 100mL.Add isopyknic petroleum ether extraction in the concentrate to slough fat.In boiling water bath, continue to be concentrated into dried after the degreasing, obtain the sticky paste of brownish black.With the paste volume ratio is 1: 5 acetone solution, filters, and repeats 2 times, merges collection filtrate.Filtrate decompression is concentrated into 20mL, and vacuum drying under 45 ℃ of conditions promptly gets the bacteriostatic agent finished product.
Embodiment 3:
Take by weighing the acorn 50g of 60 ℃ of oven dry, add 40% methanol solution 150mL, in the 250mL round-bottomed flask, filter behind 90 ℃ of water-bath backflow 4h, the leaching liquor vacuum is concentrated into 50mL according to 1: 15 solid-to-liquid ratio.Add isopyknic petroleum ether extraction in the concentrate to slough fat.In boiling water bath, continue to be concentrated into dried after the degreasing, obtain sticky paste.With the paste volume ratio is 1: 10 acetone solution, filters, and repeats 2 times, merges collection filtrate.Filtrate decompression is concentrated into 20mL, and vacuum drying under 30 ℃ of conditions promptly gets the bacteriostatic agent finished product.
In order to improve extraction efficiency, also can adopt microwave or ultrasonic-wave assisted carrying, to reach higher product yield; The dissolving of concentrate also can adopt ethyl acetate or carrene to extract.
Embodiment 4. acorn extracts are as the external bacteriostatic experiment of bacteriostatic agent:
Adopting staphylococcus aureus, Escherichia coli is indicator bacteria.Microorganism fungus kind after will activating respectively with SPSS is made finely dispersed suspension, adjusts concentration, makes thalline or spore concentration be about 10 6Individual/mL, get the adding of 0.10mL bacteria suspension respectively and contain in the aseptic plate of 20mL aseptic culture medium, the spreading rod with sterilization evenly is coated with bacterium liquid then.
The acorn extract bacteria inhibitor finished product that makes in the foregoing description is made into the sample solution of 0.2g/mL, the sterilization filter paper of diameter 5mm is soaked 30min in sample solution, take out the scraps of paper and dry.Filter paper is affixed on the culture dish surface of culture medium, is inverted, cultivated 24 hours for 37 ℃, carry out bacteriostatic experiment, observe filter paper inhibition zone size on every side, the big more fungistatic effect of inhibition zone is good more, inhibition zone thinks that greater than 10mm fungistatic effect is good, and sterile distilled water is a blank.Every kind of bacterium is cooked three parallel laboratory tests, and record inhibition zone size is averaged, and measurement data is as shown in the table.
The acorn extract supplies examination bacterium fungistatic effect to two kinds
Figure BDA0000061315520000041
Experimental result shows that the acorn extract is obvious to two kinds of fungistatic effects for the examination bacterium, illustrates that the acorn extract is a kind of good natural bacteriostatic agent.

Claims (9)

1. method for preparing bacteriostatic agent is characterized in that: adopting acorn is the raw material preparing bacteriostatic agent, and its concrete steps are:
(1) fresh acorn is cleaned impurity elimination;
(2) when bake out temperature is 40 ℃-80 ℃, dry, be milled to the acorn powder;
(3) add and to carry out carrying out after the lixiviate water-bath in the methanol solution and reflux and obtain leaching liquor;
(4) after being concentrated, leaching liquor obtains concentrate;
(5) concentrate is added extract in the extract and sloughs fat,
(6) in boiling water bath, continue to be concentrated into the dried paste that obtains after the degreasing,
(7) paste is added the acetone soln dissolving, extract 2-4 time, filter, merging filtrate, concentrate drying promptly get the acorn extract, and this acorn extract is bacteriostatic agent.
2. method according to claim 1, it is characterized in that: described acorn is the general name of Fagaceae vegetable seeds, comprises chinquapin, Mao Li, little red evergreen chinquapin, cork oak, bitter sweet oak, struggle against lithocarpus glaber, southeast lithocarpus glaber, U.S. leaf lithocarpus glaber, the lithocarpus glaber that comes into leaves, Duo Mai Qinggang, spire Qinggang, Da Ye Qinggang firmly.
3. method according to claim 1 is characterized in that: the degree of grinding of described acorn powder is the 30-100 order.
4. method according to claim 1 is characterized in that: the concentration of described methanol solution is 40%-80%, during lixiviate and the solid-to-liquid ratio of acorn powder be 1: 3-1: 15.
5. method according to claim 1 is characterized in that: the temperature that described water-bath refluxes is 70-90 ℃, and return time is 2h-4h.
6. method according to claim 1 is characterized in that: described extract is benzinum, ethyl acetate or dichloromethane solution, and wherein the volume ratio of extract and concentrate is 1: 1.
7. method according to claim 1 is characterized in that: the volume ratio of described acetone soln and dope is 1: 2-1: 10.
8. method according to claim 1 is characterized in that: described filtrate method for concentration is that normal pressure or decompression concentrate, and dry is vacuum drying, and baking temperature is 30-50 ℃.
9. the acorn extract is as the application of bacteriostatic agent.
CN 201110126437 2011-05-16 2011-05-16 Method for preparing bacteriostat and application of acorn extract used as bacteriostat Expired - Fee Related CN102240059B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102584916A (en) * 2011-12-21 2012-07-18 浙江大学 Lignan triglucoside compound and preparation method and application thereof
CN108214774A (en) * 2018-01-08 2018-06-29 西北农林科技大学 A kind of softwood sources timber preservative and preparation method thereof
CN108904625A (en) * 2018-07-26 2018-11-30 上海沃必盛生物科技有限公司 A kind of pure plant children disinfectant and its application method
CN112425711A (en) * 2020-11-23 2021-03-02 东北林业大学 Acorn shell extract coating preservative and preparation method thereof

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CN1137530A (en) * 1996-04-26 1996-12-11 泰安市泰山林场 Method for extracting edible starch from acorn and its usage
CN101747990A (en) * 2008-12-15 2010-06-23 胡景波 Preparation method of acorn oil

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Publication number Priority date Publication date Assignee Title
CN1137530A (en) * 1996-04-26 1996-12-11 泰安市泰山林场 Method for extracting edible starch from acorn and its usage
CN101747990A (en) * 2008-12-15 2010-06-23 胡景波 Preparation method of acorn oil

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102584916A (en) * 2011-12-21 2012-07-18 浙江大学 Lignan triglucoside compound and preparation method and application thereof
CN102584916B (en) * 2011-12-21 2014-01-15 浙江大学 Lignan triglucoside compound and preparation method and application thereof
CN108214774A (en) * 2018-01-08 2018-06-29 西北农林科技大学 A kind of softwood sources timber preservative and preparation method thereof
CN108904625A (en) * 2018-07-26 2018-11-30 上海沃必盛生物科技有限公司 A kind of pure plant children disinfectant and its application method
CN112425711A (en) * 2020-11-23 2021-03-02 东北林业大学 Acorn shell extract coating preservative and preparation method thereof
CN112425711B (en) * 2020-11-23 2023-01-24 东北林业大学 Acorn shell extract coating preservative and preparation method thereof

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