CN101401592A - Extracting method for kuh-seng disinfection composition and sanitizer containing the kuh-seng disinfection composition - Google Patents
Extracting method for kuh-seng disinfection composition and sanitizer containing the kuh-seng disinfection composition Download PDFInfo
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- CN101401592A CN101401592A CNA200810225645XA CN200810225645A CN101401592A CN 101401592 A CN101401592 A CN 101401592A CN A200810225645X A CNA200810225645X A CN A200810225645XA CN 200810225645 A CN200810225645 A CN 200810225645A CN 101401592 A CN101401592 A CN 101401592A
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Abstract
The invention belongs to the field of disinfectants, and in particular relates to a method for extracting a sophora flavescens bactericidal component, as well as a disinfectant prepared from sophora flavescens extract containing the sophora flavescens bactericidal component. The extraction method comprises the following steps: after dried ground sophora flavescens is added to acetone and soaked, acetone solvent for soaking the sophora flavescens is heated and refluxed; sophora flavescens dregs are filtered and removed, and then a filtrate is collected; the obtained sophora flavescens dregs are washed with the acetone, so as to obtain a washing solution; the washing solution is combined with the obtained filtrate, so as to obtain a primary filtrate; the primary filtrate is filtered by use of an ultrafiltration device and a film with the interception molecular weight between 5,000 and 10,000, so as to obtain a secondary filtrate; the obtained secondary filtrate is put into a rotary evaporator to steam off the acetone solvent, so as to obtain the sophora flavescens extract; and the sophora flavescens extract contains the effective bactericidal component of the sophora flavescens. The disinfectant which is prepared by adding acetone and alkylphenol polyoxyethylene ether as an emulsifier in certain proportion to the sophora flavescens extract contains the sophora flavescens bactericidal component and has good sterilization effects.
Description
Technical field
The invention belongs to the disinfectant field, particularly a kind of extracting method of kuh-seng sterilization composition reaches the disinfectant by the shrubby sophora extract preparation that contains kuh-seng sterilization composition of extracting.
Technical background
In the bactericide that present stage uses, chemicals occupies sizable ratio, and the long-term use of chemicals has brought problems such as chemicals is residual, environmental pollution to environment.Under the situation that global environmental consciousness strengthens, chemicals is being faced with serious challenge, derives from the focus that natural medicine is just becoming drug development research.Derive from natural medicine and comprise and come from plant resource, microbial source and mineral sources medicine that wherein major part is the medicine that derives from plant.Most of secondary metabolites in the plant such as terpenes, alkaloids, flavonoids, black body, phenols and special acid, polysaccharide etc. all have antibiotic, bacteriostatic activity.The Chinese herbal medicine source bactericide is to utilize the traditional Chinese medicine extraction technology, and the composition with bactericidal action is extracted from Chinese herbal medicine, obtains the monomeric substance of separation and purification.These compositions are that nature exists, and generally are easy to degraded, and are little to environment savings toxicity possibility, compare with the bactericide of chemical composition, the bactericide in Chinese medicine medicine source is lower to the toxicity of humans and animals, and is less to the influence of ecotope, is very promising environment-friendly type medicine.
In extracting method, heat reflow method is to be solvent with volatile organic solvent, and leachate is added thermal distillation.By the evaporation and the backflow of organic solvent, make that the solvent that at every turn contacts with raw material all is pure organic solvent, improve extraction power, thereby improved rate of extraction and effect.The method is used comparatively extensively in effective components of Chinese medicinal is extracted, and existing literature has more report.But extract by heat reflow method, contain relative molecular mass in the extract greater than several ten thousand impurity (invalid element), the existence of this part impurity has destroyed the effect of effective ingredient.
Summary of the invention
The objective of the invention is the problem that exists in the existing hot reflux technology, a kind of simple, effective extracting method of kuh-seng sterilization composition is provided.
Another object of the present invention is to provide a kind of bactericidal effect good, contain the disinfectant of kuh-seng sterilization composition.
The extracting method of kuh-seng sterilization composition of the present invention may further comprise the steps:
1) to join be to soak after 24 hours in the acetone of its 8～10 times of weight to the kuh-seng of getting drying and crushing, and the acetone solvent that soaks kuh-seng was added hot reflux 1.5～2 hours, then the kuh-seng slag removed by filter, and collects filtrate;
2) the kuh-seng slag of using the washing with acetone step 1) with the step 1) identical weight to obtain obtains cleaning solution, and the filtrate that cleaning solution and step 1) are obtained merges, and this is a first-time filtrate;
3) utilize ultrafiltration apparatus, adopting the intercepting molecular weight is 5000～10000 membrane filtration step 2) first-time filtrate that obtains, obtain secondary filtrate; The secondary filtrate that obtains is put into Rotary Evaporators, steam solvent acetone, obtain shrubby sophora extract, the effective sterilization composition that contains kuh-seng in this shrubby sophora extract, the mass content of effective sterilization composition of kuh-seng is about 96% (table 1), the shrubby sophora extract that obtains is pulverized the back be the sundown powder.
Effective sterilization composition of described shrubby sophora extract is a matrine.
The disinfectant that contains kuh-seng sterilization composition that the shrubby sophora extract that contains kuh-seng sterilization composition that utilizes method of the present invention to obtain prepares:
Adding acetone and emulsifier nonyl phenol polyethenoxy ether (TX-10) are mixed with the disinfectant that contains kuh-seng sterilization composition in shrubby sophora extract; Wherein, contain shrubby sophora extract 3～5 weight % in the disinfectant, surplus is acetone and emulsifier TX-10, and the volume ratio of acetone and emulsifier TX-10 is 1: 1.
Adopt acetone extraction, secondary filter method to obtain having the shrubby sophora extract of bactericidal action among the present invention.In the filtrate filtration test, adopt a series of filter methods, utilized gas chromatography that filtrate is carried out qualitative, quantitative analysis, the results are shown in Table 1.
The extraction result of the different filter methods of table 1.
| Filter method | The filtrate color | Recovery rate (%) | The mass content (%) of effective sterilization composition | The extract proterties |
| Once filter | Dark brown red | 13.9 | 75 | The thickness oily |
| Ultrafiltration (retaining molecular weight 70,000) | Brownish red | 12.8 | 81 | The thickness oily |
| Ultrafiltration (film intercepting molecular weight 50,000) | Brownish red | 12.4 | 84 | The thickness oily |
| Ultrafiltration (film intercepting molecular weight 20,000) | Brownish red | 11.9 | 88 | Gu shape |
| Ultrafiltration (film intercepting molecular weight 5000～10000) | Sundown | 10.8 | 96 | Gu shape is frangible |
By the analysis of gas chromatography to filtrate, the result shows the first-time filtrate that does not adopt ultrafiltration to filter, collection of illustrative plates (Fig. 1) impurity peaks is many, and adopt ultrafiltration that first-time filtrate is filtered, reduction along with film intercepting molecular weight, impurity peaks reduces gradually, and effective component content in the extract (mass ratio) improves.Adopt the film of intercepting molecular weight 5000～10000 that first-time filtrate is carried out ultrafiltration, this condition the best, it is the highest to obtain the extract effective component content, impurity peaks little (Fig. 2).
The extracting method of kuh-seng sterilization composition of the present invention is a kind of extracting method of simple, effective kuh-seng sterilization composition.The disinfectant that contains kuh-seng sterilization composition that the shrubby sophora extract that contains kuh-seng sterilization composition that utilizes method of the present invention to obtain prepares, in bactericidal assay, the disinfectant that shrubby sophora extract is mixed with all reaches 99.9% to the sterilizing rate of Escherichia coli and golden staphylococci, is respond well disinfectant.
Description of drawings
Fig. 1. the first-time filtrate gas chromatogram of the embodiment of the invention 2.
Fig. 2. the secondary filtrate gas chromatogram of the embodiment of the invention 2.
Embodiment
Get the kuh-seng that 200g pulverizes, be placed in the drying box fully drying after, joining is to soak after 24 hours in the acetone of its 8 times of weight, and the acetone solvent that soaks kuh-seng was added hot reflux 1.5 hours, then with the filtering of kuh-seng slag, collects filtrate; The kuh-seng slag that obtains with the washing with acetone of weight same as described above once obtains cleaning solution, and cleaning solution and the above-mentioned filtrate that obtains are merged, and this is a first-time filtrate.Utilize ultrafiltration apparatus, employing intercepting molecular weight is 5000～10000 polyether sulfone (PES) membrane filtration first-time filtrate, obtains secondary filtrate; The secondary filtrate that obtains is put into Rotary Evaporators, steam solvent acetone under the condition of-0.01Mpa and 40 ℃, obtain shrubby sophora extract, pulverizing the back is the sundown powder.The effective sterilization composition that contains kuh-seng in this shrubby sophora extract, the mass content of effective sterilization composition of kuh-seng are about 96% (seeing Table the result of film intercepting molecular weight 5000～10000 in 1).
The shrubby sophora extract that embodiment 1 method is obtained carries out gas-chromatography separation and mensuration.
The shrubby sophora extract acetone solution uses XE-60 (25m, 0.25mm, 0.25 μ m) quartz capillary chromatographic column and fid detector to carry out gas-chromatography and separates and measure, and the result as illustrated in fig. 1 and 2.
Prepare disinfectant with the shrubby sophora extract that embodiment 1 method obtains.
Get 3g shrubby sophora extract powder, add 50ml acetone and 50ml emulsifier TX-10 therein, fully shake up, obtain pale-yellow emulsion, be the disinfectant that content is 3 weight %.
The disinfectant of the shrubby sophora extract preparation that obtains with embodiment 3.
Get respectively staphylococcus aureus ATCC 6538, Escherichia coli 8099 the 3rd generation～the 14th generation the nutrient agar slant tube fresh cultured thing (incubation time 18 hours～24 hours), drawing 3.0ml～5.0ml dilution (dilution is the normal saline solution of 0.1% tryptone) with the 5.0ml suction pipe adds in the slant tube, pressure-vaccum repeatedly, wash the lawn in the slant tube, with the 5.0ml suction pipe bacterium liquid that washes is moved in another sterile test tube subsequently, with electronic mixing 20 seconds, make bacteria suspension.Measure bacteria suspension concentration with the bacterial concentration nephelometry earlier, using dilution (dilution is the normal saline solution of 0.1% tryptone) to be diluted to concentration then is 5 * 10
6～5 * 10
7Cfu/ml gets the bacteria suspension 0.5ml after the dilution, adds 0.5ml organic matter interfering material (3% (W/V) bovine serum albumin(BSA)) mixing again, then test tube is placed 20 ℃ ± 1 ℃ water-bath 5 minutes.Draw in the 4.0ml disinfectant injecting tube, mixing clocks, wait to act on to stipulated time (positive control is a dilution), get the mixed liquor of 0.5ml disinfectant and bacterium again, add 4.5ml neutralizer (mass concentration is that 1% lecithin+mass concentration is the aqueous solution of 1% Tween 80) in test tube, neutralization 10 minutes, draw 1.0ml inoculation plate, do colony counting, calculate killing rate, sterilizing rate is 99.9%.
Get the kuh-seng that 200g pulverizes, be placed in the drying box fully drying after, joining is to soak after 24 hours in the acetone of its 8 times of weight, and the acetone solvent that soaks kuh-seng was added hot reflux 2 hours, then with the filtering of kuh-seng slag, collects filtrate; The kuh-seng slag that obtains with the washing with acetone of weight same as described above once obtains cleaning solution, and cleaning solution and the above-mentioned filtrate that obtains are merged, and this is a first-time filtrate.Utilize ultrafiltration apparatus, employing intercepting molecular weight is 5000～10000 polyether sulfone (PES) membrane filtration first-time filtrate, obtains secondary filtrate; The secondary filtrate that obtains is put into Rotary Evaporators, steam solvent acetone under the condition of-0.01Mpa and 40 ℃, obtain shrubby sophora extract, pulverizing the back is the sundown powder.
Embodiment 6
Get the kuh-seng that 200g pulverizes, be placed in the drying box fully drying after, joining is to soak after 24 hours in the acetone of its 10 times of weight, and the acetone solvent that soaks kuh-seng was added hot reflux 2 hours, then with the filtering of kuh-seng slag, collects filtrate; The kuh-seng slag that obtains with the washing with acetone of weight same as described above once obtains cleaning solution, and cleaning solution and the above-mentioned filtrate that obtains are merged, and this is a first-time filtrate.Utilize ultrafiltration apparatus, employing intercepting molecular weight is 5000～10000 polyether sulfone (PES) membrane filtration first-time filtrate, obtains secondary filtrate; The secondary filtrate that obtains is put into Rotary Evaporators, steam solvent acetone under the condition of-0.01Mpa and 40 ℃, obtain shrubby sophora extract, pulverizing the back is the sundown powder.
Embodiment 7
Prepare disinfectant with the shrubby sophora extract that embodiment 6 methods obtain.
Get 3g shrubby sophora extract powder, add 50ml acetone and 50ml emulsifier TX-10 therein, fully shake up, obtain pale-yellow emulsion, be the disinfectant that content is about 5 weight %.
Claims (4)
1. the extracting method of a kuh-seng sterilization composition is characterized in that, this method may further comprise the steps:
1) to join be to soak after 24 hours in the acetone of its 8～10 times of weight to the kuh-seng of getting drying and crushing, and the acetone solvent that soaks kuh-seng was added hot reflux 1.5～2 hours, then the kuh-seng slag removed by filter, and collects filtrate;
2) the kuh-seng slag of using the washing with acetone step 1) with the step 1) identical weight to obtain obtains cleaning solution, and the filtrate that cleaning solution and step 1) are obtained merges, and this is a first-time filtrate;
3) utilize ultrafiltration apparatus, adopting the intercepting molecular weight is 5000～10000 membrane filtration step 2) first-time filtrate that obtains, obtain secondary filtrate; The secondary filtrate that obtains is put into Rotary Evaporators, steam solvent acetone, obtain shrubby sophora extract, contain effective sterilization composition of kuh-seng in this shrubby sophora extract.
2. method according to claim 1 is characterized in that: effective sterilization composition of described shrubby sophora extract is a matrine.
3. disinfectant that contains kuh-seng sterilization composition that utilizes the shrubby sophora extract preparation that contains kuh-seng sterilization composition that claim 1 or 2 obtains is characterized in that:
Adding acetone and emulsifier nonyl phenol polyethenoxy ether are mixed with the disinfectant that contains kuh-seng sterilization composition in shrubby sophora extract; Wherein, contain shrubby sophora extract 3～5 weight % in the disinfectant, surplus is acetone and emulsifier nonyl phenol polyethenoxy ether, and the volume ratio of acetone and emulsifier nonyl phenol polyethenoxy ether is 1: 1.
4. disinfectant according to claim 3 is characterized in that: described disinfectant is 99.9% to golden staphylococci and colibacillary killing rate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810225645XA CN101401592A (en) | 2008-11-03 | 2008-11-03 | Extracting method for kuh-seng disinfection composition and sanitizer containing the kuh-seng disinfection composition |
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| CNA200810225645XA CN101401592A (en) | 2008-11-03 | 2008-11-03 | Extracting method for kuh-seng disinfection composition and sanitizer containing the kuh-seng disinfection composition |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102578111A (en) * | 2012-01-12 | 2012-07-18 | 中国检验检疫科学研究院 | Disinfectant and preparation method thereof |
| CN103271985A (en) * | 2013-06-14 | 2013-09-04 | 柯美华 | Disinfectant for skin and mucosa |
| CN103739602A (en) * | 2013-12-16 | 2014-04-23 | 广西大学 | Method for extracting matrine |
| CN105053043A (en) * | 2015-08-26 | 2015-11-18 | 湖州旭龙生物化学有限公司 | Sterilization composition containing kresoxim-methyl and radix sophorae flavescentis extract |
-
2008
- 2008-11-03 CN CNA200810225645XA patent/CN101401592A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102578111A (en) * | 2012-01-12 | 2012-07-18 | 中国检验检疫科学研究院 | Disinfectant and preparation method thereof |
| CN103271985A (en) * | 2013-06-14 | 2013-09-04 | 柯美华 | Disinfectant for skin and mucosa |
| CN103739602A (en) * | 2013-12-16 | 2014-04-23 | 广西大学 | Method for extracting matrine |
| CN105053043A (en) * | 2015-08-26 | 2015-11-18 | 湖州旭龙生物化学有限公司 | Sterilization composition containing kresoxim-methyl and radix sophorae flavescentis extract |
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Open date: 20090408 |