CN104018343B - A kind of Chinese fiber crops bast fiber extract, preparation method and its usage with antibacterial activity - Google Patents
A kind of Chinese fiber crops bast fiber extract, preparation method and its usage with antibacterial activity Download PDFInfo
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Abstract
The present invention relates to a kind of Chinese fiber crops bast fiber extract, preparation method and its usage.Described extracting method comprises the steps: that raw material is washed by (1); (2) dry, shred; (3) Solvent Extract methods; (4) reduced pressure concentration, obtains primary extract medicinal extract; (5) primary extract medicinal extract is carried out the liquid-liquid extraction using mineral solution and organic solvent, obtain medicinal extract; (6) medicinal extract is loaded in silica gel column chromatography, organic solvent wash-out, collect eluent, reduced pressure concentration, obtain described Chinese fiber crops bast fiber extract.This extract has excellent broad-spectrum antimicrobial effect, can be used as natural antibacterial finishing agent and is applied in the processes such as the antibiotic finish of textiles.Described extract of the present invention, extracting method and uses thereof have industrial application value and market prospects very widely.
Description
Technical field
The present invention relates to a kind of extract, preparation method and its usage of string active component, relate more particularly to a kind of Chinese fiber crops bast fiber extract, the preparation method and its usage with antibacterial activity, belong to Chinese fiber crops comprehensive utilization technique and textile application field.
Background technology
Industrial hemp (CannabisSativaL.) is a kind of fibre of flax for textile material having economic worth, people are by the improvement of genes to hemp, reduce its toxic component (tetrahydrocannabinol THC content is lower than 0.3%), obtain the low toxicity hemp-Han fiber crops of green safety more.
China is the main product state of Chinese fiber crops, planting area throughout North China, northwest, East China, multiple area such as Central-South, output accounts for about 1/3 of world's hemp output, ranks first in the world.Rich in natural resources deposit is that the exploitation of China's Chinese fiber crops industry provides strong support.
The numb characteristic excellent because of its each side of the Chinese and function, be widely used in contemporary textile industry.In recent years the research of chemical composition in Chinese fiber crops plant is mainly carried out from the Chinese fiber crops leaf and the aspect such as chemical composition, chemical composition route of synthesis and chemical moiety activity had the Chinese fiber crops seed of edibility with medical value.Based on medical value, part document also considers that the chemical composition to the leaf part in Chinese fiber crops plant mixes is extracted, and carried out tracking, Isolation and screening to its antibacterial chemical composition.
The people such as Zhou Yongkai (" the female person of outstanding talent of hemp emerging and antibacterial mechanisms ", " textile journal ", 28 volumes the 6th phase, in June, 2007) hemp is studied, after hemp bast fiber being carried out high-temperature sterilization, cooling, still to various bacteria, there is good antibacterial and inhibitory action.
The people such as Zhang Gang (extraction process of cannabinol compounds " in the preferred fructus cannabis oil of orthogonal experiment ", " Chinese medicine ", 28th volume the 5th phase, in May, 2005) disclose the method extracting active component in cannabis,fructus oil, the method by using the materials such as methyl alcohol ultrasonic extraction cannabinol, have recovery rate high, save time, the advantage such as energy-conservation.
The people such as Cheng Liang (" petroleum ether extraction of industrial hemp research .I. methanolic extract and the chemical composition of n-butanol portion ", " Chinese Journal of Pharmaceuticals ", 39 (1), 39 (2), 2008) by carrying out methyl alcohol extraction to industrial hemp, be separated from its petroleum ether portion and identify 14 compounds, be separated from its ethyl acetate extraction part and obtain 11 compounds.
WO2004016277A discloses the extracting method to the pharmaceutical active Cannabinoids from plant: comprise decarboxylation step, extract and reduce the step of non-targeted material proportion in extract with liquid carbon dioxide.
Disclose a kind of method extracting active constituents of medicine from hemp in GB0200620, comprise the hemp of mincing to heat under sufficient temp and carry out decarboxylation, then use CO
2carry out means of supercritical extraction, finally also cross with alcohol settling at low temperatures and filter Wax.
As mentioned above, although carried out large quantity research for hemp, mainly concentrate on leaf, planted the higher position of isoreactivity component content, and less for the active matter Quality Research had in the bast fiber of weaving value in Chinese fiber crops plant.
But then, extraction and isolation obtains the antibiotic property class material in Chinese fiber crops bast fiber, can keep the function of hemp fibre products, develop high-grade antibacterial garment product there is important directive significance, thus industrially have a good application prospect and potentiality, this also just the power place that is accomplished of the present invention and basis lean on.
Summary of the invention
In order to overcome above-mentioned pointed many defects, the present inventor is to this has been further investigation, after having paid a large amount of creative work, thus develop a kind of Chinese fiber crops bast fiber extract, the preparation method and its usage with antibacterial activity, and then complete the present invention.
Specifically, technical scheme of the present invention and content relate to a kind of Chinese fiber crops bast fiber extract, the preparation method and its usage with antibacterial activity.
First aspect, the present invention relates to the preparation method of a kind of Chinese fiber crops bast fiber extract, described method comprises the steps:
(1) raw material is washed;
(2) dry, shred;
(3) Solvent Extract methods;
(4) reduced pressure concentration, obtains primary extract medicinal extract;
(5) primary extract medicinal extract is carried out the liquid-liquid extraction using mineral solution and organic solvent, obtain medicinal extract;
(6) medicinal extract is loaded in silica gel column chromatography, organic solvent wash-out, collect eluent, reduced pressure concentration, obtain described Chinese fiber crops bast fiber extract.
In the preparation method of Chinese fiber crops bast fiber extract of the present invention, raw material in described step (1) is the bast fiber (below sometimes also referred to as " Chinese fiber crops bast fiber ") in Chinese straw, carried out normal temperature washing, wash away surface irregularities and/or dirt, thus obtain clean Chinese fiber crops bast fiber.
In the preparation method of Chinese fiber crops bast fiber extract of the present invention, in described step (2), by the clean Chinese fiber crops bast fiber vacuumize or natural air drying at 40-80 DEG C, then shredded, such as can shred into area and be less than 1cm × 1cm, certainly this is exemplary exemplifying, and also can be shredded the thinner fritter of Cheng Geng little.
In the preparation method of Chinese fiber crops bast fiber extract of the present invention, described step (3) concrete operations are as follows: in the Chinese fiber crops bast fiber after shredding, add organic solvent, stir at 60-90 DEG C and extract 2-4 hour, filter and collect filtrate after extracting.
Wherein, described organic solvent is the lower alcohol with 1-6 carbon atom, such as can be any one in methyl alcohol, ethanol, normal propyl alcohol, isopropyl alcohol, n-butanol, n-amyl alcohol, n-hexyl alcohol or multiple mixture in non-limiting manner.
Wherein, by weight, described organic solvent with shred after the Chinese fiber crops bast fiber ratio be 10-20:1, such as can be 10:1,15:1 or 20:1.
Wherein, Extracting temperature is 60-90 DEG C, such as can be 60 DEG C, 70 DEG C, 80 DEG C or 90 DEG C in non-limiting manner.
Wherein, extraction time is 2-4 hour, such as can be 2 hours in non-limiting manner, 3 hours or 4 hours.
It should be noted that this Solvent Extract methods process can carry out 1 time, or repeat 2-4 time.Specifically, such as 1 time, 2 times, 3 times or 4 times can be carried out.
In the preparation method of Chinese fiber crops bast fiber extract of the present invention, described step (4) concrete operations are: the filtrate of step (3) gained is carried out reduced pressure concentration, except desolventizing, obtain primary extract medicinal extract.
Wherein, there is no particular limitation for the mode of reduced pressure concentration, such as, Rotary Evaporators can be used to carry out reduced pressure concentration process, thus by solvent evaporation removing, obtain primary extract medicinal extract.
In the preparation method of Chinese fiber crops bast fiber extract of the present invention, the mineral solution in described step (5) is the NaCl aqueous solution, is preferably the saturated NaCl aqueous solution.
In the preparation method of Chinese fiber crops bast fiber extract of the present invention, the organic solvent in described step (5) is ethyl acetate.
More preferably, described step (5) concrete operations are as follows: fully shaken up by the saturated NaCl aqueous solution of primary extract medicinal extract, dissolve, suction filtration, obtain aqueous phase and non-dissolved solid; Non-dissolved solid ethyl acetate is fully shaken up, dissolves, obtains ethyl acetate phase; Described aqueous phase and ethyl acetate are added in separatory funnel, fully shake up, mix, stratification, aqueous phase discarded, by ethyl acetate phase reduced pressure concentration, obtain ethyl acetate phase medicinal extract.
Wherein, the saturated NaCl aqueous solution is 10-20:1ml/g with the volume mass ratio of primary extract medicinal extract, namely every 1g just extracts medicinal extract and uses the 10-20ml saturated NaCl aqueous solution to process, such as, can be 10:1ml/g, 12:1ml/g, 14:1ml/g, 16:1ml/g, 18:1ml/g or 20:1ml/g.
Wherein, ethyl acetate is 5-10:1ml/g with the volume mass ratio of described non-dissolved solid, namely the non-dissolved solid of every 1g uses 5-10ml ethyl acetate to process, such as, can be 5:1ml/g, 6:1ml/g, 7:1ml/g, 8:1ml/g, 9:1ml/g or 10:1ml/g.
In the preparation method of Chinese fiber crops bast fiber extract of the present invention, described step (6) concrete operations are as follows: fully dissolved by ethyl acetate phase medicinal extract chloroform, and to join granularity be in 200-300 object silica gel, stir, obtain silica gel absorption sample; Described silica gel absorption sample is joined the silica gel column chromatography top filled, then with an organic solvent wash-out is carried out, started to collect eluent by time bottom solvent washing to chromatographic column until sample, collect the eluent being equivalent to 2-4 column volume, by this eluent reduced pressure concentration, obtain described Chinese fiber crops bast fiber extract.
Wherein, the chloroform dissolving described ethyl acetate phase medicinal extract is 1-2:1 with the mass ratio of ethyl acetate phase medicinal extract, such as, can be 1:1,1.5:1 or 2:1.
Wherein, the described organic solvent carrying out wash-out is the mixture of chloroform and methyl alcohol, and wherein the volume ratio of chloroform and methyl alcohol is 46-50:1, such as, can be 46:1,47:1,48:1,49:1 or 50:1.
Preferably, acetone is added in the organic solvent of above-mentioned wash-out, namely preferred, the described organic solvent carrying out wash-out is the mixture of chloroform, methyl alcohol and acetone, wherein the volume ratio of chloroform, methyl alcohol, acetone is 46-50:1:2-4, such as can be 46:1:2,47:1:2,48:1:2,49:1:2,50:1:2,46:1:3,47:1:3,48:1:3,49:1:3,50:1:3,46:1:4,47:1:4,48:1:4,49:1:4 or 50:1:4, be preferably 46-50:1:3.
Inventor finds, when adding acetone, the anti-microbial property of the Chinese fiber crops bast fiber extract obtained improves further, has more excellent effect.
Wherein, described silica gel column chromatography fills post as follows: be soaked in chloroform by 200-300 object silica gel, and fully swelling, till no longer swelling, then fills post, and sedimentation one is late.
Second aspect, the present invention relates to the Chinese fiber crops bast fiber extract prepared by said method.
The present inventor is found by research, and described Chinese fiber crops bast fiber extract of the present invention has excellent broad-spectrum antimicrobial effect, can be used as natural antibacterial finishing agent and is applied in the processes such as the antibiotic finish of textiles.
Therefore, the 3rd aspect, the present invention relates to the purposes of described Chinese fiber crops bast fiber extract in textile field.
In described purposes of the present invention, described purposes is the antibacterial finishing agent being used as textiles.
Compared with prior art, beneficial effect of the present invention is:
1, the inventive method is extracted by selecting suitable organic solvent, thus can effectively be extracted by antimicrobial component.
2, the inventive method is by adopting liquid-liquid extraction, is enriched active ingredient further.
3, the inventive method is by suitable column chromatography technological parameter and the means such as the selection of eluting solvent, the selection of suitable silica gel, thus can obtain the Chinese fiber crops bast fiber antibiotic effective ingredient with excellent antibacterial effect.
4, by using the mixing eluting solvent system of chloroform, methyl alcohol and acetone, the bast fiber extract with excellent antibacterial performance can be obtained.
Detailed description of the invention
Below by specific embodiment, the present invention is described in detail; but the purposes of these exemplary embodiments and object are only used for exemplifying the present invention; not any type of any restriction is formed to real protection scope of the present invention, more non-protection scope of the present invention is confined to this.
Preparation example 1: silica gel adsorption column dress post
200-300 object silica gel is soaked in chloroform, and fully swelling, till no longer swelling, then fill post, and sedimentation one is late, obtains silicagel column.
Unless otherwise specified, the silicagel column used in all embodiments below, to be in this preparation example 1 load the silicagel column obtained.
Preparation example 2: silica gel adsorption column dress post
200-300 object silica gel is directly filled post, and sedimentation one is late, obtains silicagel column, does not namely use chloroform to carry out fully swelling.
Embodiment 1
(1) Chinese fiber crops bast fiber is carried out normal temperature washing, wash away surface irregularities and/or dirt, thus obtain clean Chinese fiber crops bast fiber.
(2) by the vacuumize at 40 DEG C of clean Chinese fiber crops bast fiber, the fritter that area is less than 1cm × 1cm is then shredded into.
(3) in the Chinese fiber crops bast fiber after shredding, be incorporated as the ethanol of Chinese fiber crops bast fiber weight 10 times of weight, extraction is stirred 4 hours at 60 DEG C, this leaching process can carry out 1 time or 2-4 time, filter and collect filtrate (when carrying out repeatedly, each filtrate being merged) after extracting.
(4) use Rotary Evaporators that the filtrate of step (3) gained is carried out reduced pressure concentration, except desolventizing, obtain primary extract medicinal extract.
(5) the saturated NaCl aqueous solution of primary extract medicinal extract fully shaken up, dissolve, suction filtration, obtain aqueous phase and non-dissolved solid; Non-dissolved solid ethyl acetate is fully shaken up, dissolves, obtains ethyl acetate phase; Described aqueous phase and ethyl acetate are added in separatory funnel, fully shake up, mix, stratification, aqueous phase discarded, by ethyl acetate phase reduced pressure concentration, obtain ethyl acetate phase medicinal extract.
Wherein, the saturated NaCl aqueous solution and the volume mass of primary extract medicinal extract are than being 10:1ml/g; Ethyl acetate is 5ml/g with the volume mass ratio of described non-dissolved solid.
(6) ethyl acetate phase medicinal extract chloroform is fully dissolved, and to join granularity be in 200-300 object silica gel, stir, obtain silica gel absorption sample; Described silica gel absorption sample is joined the preparation example 1 silicagel column top filled, then the mixed organic solvents of chloroform and methyl alcohol is used to carry out wash-out, started to collect elute soln by time bottom solvent washing to chromatographic column until sample, collect the elute soln being equivalent to 2 column volumes, by this elute soln reduced pressure concentration, obtain described Chinese fiber crops bast fiber extract, called after XW1.
Wherein, the chloroform dissolving described ethyl acetate phase medicinal extract is 1:1 with the mass ratio of ethyl acetate phase medicinal extract; The volume ratio of the chloroform and methyl alcohol that carry out wash-out is 46:1.
Embodiment 2
(1) Chinese fiber crops bast fiber is carried out normal temperature washing, wash away surface irregularities and/or dirt, thus obtain clean Chinese fiber crops bast fiber.
(2) by the vacuumize at 60 DEG C of clean Chinese fiber crops bast fiber, the fritter that area is less than 1cm × 1cm is then shredded into.
(3) in the Chinese fiber crops bast fiber after shredding, be incorporated as the ethanol of Chinese fiber crops bast fiber weight 15 times of weight, extraction is stirred 3 hours at 70 DEG C, this leaching process can carry out 1 time or 2-4 time, filter and collect filtrate (when carrying out repeatedly, each filtrate being merged) after extracting.
(4) use Rotary Evaporators that the filtrate of step (3) gained is carried out reduced pressure concentration, except desolventizing, obtain primary extract medicinal extract.
(5) the saturated NaCl aqueous solution of primary extract medicinal extract fully shaken up, dissolve, suction filtration, obtain aqueous phase and non-dissolved solid; Non-dissolved solid ethyl acetate is fully shaken up, dissolves, obtains ethyl acetate phase; Described aqueous phase and ethyl acetate are added in separatory funnel, fully shake up, mix, stratification, aqueous phase discarded, by ethyl acetate phase reduced pressure concentration, obtain ethyl acetate phase medicinal extract.
Wherein, the saturated NaCl aqueous solution and the volume mass of primary extract medicinal extract are than being 14:1ml/g; Ethyl acetate is 7ml/g with the volume mass ratio of described non-dissolved solid.
(6) ethyl acetate phase medicinal extract chloroform is fully dissolved, and to join granularity be in 200-300 object silica gel, stir, obtain silica gel absorption sample; Described silica gel absorption sample is joined the preparation example 1 silicagel column top filled, then the mixed organic solvents of chloroform and methyl alcohol is used to carry out wash-out, started to collect elute soln by time bottom solvent washing to chromatographic column until sample, collect the elute soln being equivalent to 3 column volumes, by this elute soln reduced pressure concentration, obtain described Chinese fiber crops bast fiber extract, called after XW2.
Wherein, the chloroform dissolving described ethyl acetate phase medicinal extract is 1.5:1 with the mass ratio of ethyl acetate phase medicinal extract; The volume ratio of the chloroform and methyl alcohol that carry out wash-out is 48:1.
Embodiment 3
(1) Chinese fiber crops bast fiber is carried out normal temperature washing, wash away surface irregularities and/or dirt, thus obtain clean Chinese fiber crops bast fiber.
(2) by the vacuumize at 80 DEG C of clean Chinese fiber crops bast fiber, the fritter that area is less than 1cm × 1cm is then shredded into.
(3) in the Chinese fiber crops bast fiber after shredding, be incorporated as the ethanol of Chinese fiber crops bast fiber weight 20 times of weight, extraction is stirred 2 hours at 80 DEG C, this leaching process can carry out 1 time or 2-4 time, filter and collect filtrate (when carrying out repeatedly, each filtrate being merged) after extracting.
(4) use Rotary Evaporators that the filtrate of step (3) gained is carried out reduced pressure concentration, except desolventizing, obtain primary extract medicinal extract.
(5) the saturated NaCl aqueous solution of primary extract medicinal extract fully shaken up, dissolve, suction filtration, obtain aqueous phase and non-dissolved solid; Non-dissolved solid ethyl acetate is fully shaken up, dissolves, obtains ethyl acetate phase; Described aqueous phase and ethyl acetate are added in separatory funnel, fully shake up, mix, stratification, aqueous phase discarded, by ethyl acetate phase reduced pressure concentration, obtain ethyl acetate phase medicinal extract.
Wherein, the saturated NaCl aqueous solution and the volume mass of primary extract medicinal extract are than being 17:1ml/g; Ethyl acetate is 8ml/g with the volume mass ratio of described non-dissolved solid.
(6) ethyl acetate phase medicinal extract chloroform is fully dissolved, and to join granularity be in 200-300 object silica gel, stir, obtain silica gel absorption sample; Described silica gel absorption sample is joined the preparation example 1 silicagel column top filled, then the mixed organic solvents of chloroform and methyl alcohol is used to carry out wash-out, started to collect elute soln by time bottom solvent washing to chromatographic column until sample, collect the elute soln being equivalent to 4 column volumes, by this elute soln reduced pressure concentration, obtain described Chinese fiber crops bast fiber extract, called after XW3.
Wherein, the chloroform dissolving described ethyl acetate phase medicinal extract is 2:1 with the mass ratio of ethyl acetate phase medicinal extract; The volume ratio of the chloroform and methyl alcohol that carry out wash-out is 50:1.
Embodiment 4
(1) Chinese fiber crops bast fiber is carried out normal temperature washing, wash away surface irregularities and/or dirt, thus obtain clean Chinese fiber crops bast fiber.
(2) by the vacuumize at 50 DEG C of clean Chinese fiber crops bast fiber, the fritter that area is less than 1cm × 1cm is then shredded into.
(3) in the Chinese fiber crops bast fiber after shredding, be incorporated as the ethanol of Chinese fiber crops bast fiber weight 13 times of weight, extraction is stirred 3 hours at 90 DEG C, this leaching process can carry out 1 time or 2-4 time, filter and collect filtrate (when carrying out repeatedly, each filtrate being merged) after extracting.
(4) use Rotary Evaporators that the filtrate of step (3) gained is carried out reduced pressure concentration, except desolventizing, obtain primary extract medicinal extract.
(5) the saturated NaCl aqueous solution of primary extract medicinal extract fully shaken up, dissolve, suction filtration, obtain aqueous phase and non-dissolved solid; Non-dissolved solid ethyl acetate is fully shaken up, dissolves, obtains ethyl acetate phase; Described aqueous phase and ethyl acetate are added in separatory funnel, fully shake up, mix, stratification, aqueous phase discarded, by ethyl acetate phase reduced pressure concentration, obtain ethyl acetate phase medicinal extract.
Wherein, the saturated NaCl aqueous solution and the volume mass of primary extract medicinal extract are than being 20:1ml/g; Ethyl acetate is 10ml/g with the volume mass ratio of described non-dissolved solid.
(6) ethyl acetate phase medicinal extract chloroform is fully dissolved, and to join granularity be in 200-300 object silica gel, stir, obtain silica gel absorption sample; Described silica gel absorption sample is joined the preparation example 1 silicagel column top filled, then the mixed organic solvents of chloroform and methyl alcohol is used to carry out wash-out, started to collect elute soln by time bottom solvent washing to chromatographic column until sample, collect the elute soln being equivalent to 3 column volumes, by this elute soln reduced pressure concentration, obtain described Chinese fiber crops bast fiber extract, called after XW4.
Wherein, the chloroform dissolving described ethyl acetate phase medicinal extract is 1.5:1 with the mass ratio of ethyl acetate phase medicinal extract; The volume ratio of the chloroform and methyl alcohol that carry out wash-out is 47:1.
Embodiment 5-8
Except the chloroform in step (6), methyl alcohol mixing eluting solvent are replaced with following chloroform, methyl alcohol, acetone mixed solvent as except eluting solvent, respectively to have carried out embodiment 5-8 with the same way of embodiment 1-4, obtain described Chinese fiber crops bast fiber extract called after XW5-XW8 successively, its corresponding relation, mixed solvent volume ratio see the following form shown in 1:
Table 1
Comparative example 1-12
Except using methyl alcohol in step (3) respectively and replacing ethanol, respectively to implement comparative example 1-4 with the same way of embodiment 1-4, the described Chinese fiber crops bast fiber extract called after D1-D4 successively obtained.
Except using normal propyl alcohol alcohol in step (3) respectively and replacing ethanol, respectively to implement comparative example 1-4 with the same way of embodiment 1-4, the described Chinese fiber crops bast fiber extract called after D5-D8 successively obtained.
Except using n-butanol alcohol in step (3) respectively and replacing ethanol, respectively to implement comparative example 1-4 with the same way of embodiment 1-4, the described Chinese fiber crops bast fiber extract called after D9-D12 successively obtained.
Comparative example 13-16
Fully shaking up except not using the saturated NaCl aqueous solution in step (5), dissolving, suction filtration, obtain outside aqueous phase, respectively to have carried out comparative example 13-16 with the same way of embodiment 1-4, ethyl acetate is namely directly used to carry out processing and obtaining ethyl acetate phase medicinal extract.The described Chinese fiber crops bast fiber extract called after D13-D16 successively obtained.
Comparative example 17-20
Except using the silicagel column of preparation example 2 and replacing the silicagel column of preparation example 1, respectively to have carried out comparative example 17-20 with the same way of embodiment 1-4, the described Chinese fiber crops bast fiber extract called after D17-D20 successively obtained.
Comparative example 21-28
Replace the mixed solvent of chloroform and methyl alcohol as except eluting solvent except being used alone chloroform in step (6), respectively to have carried out comparative example 21-24 with the same way of embodiment 1-4, obtain described Chinese fiber crops bast fiber extract called after D21-D24 successively.
Replace the mixed solvent of chloroform and methyl alcohol as except eluting solvent except being used alone methyl alcohol in step (6), respectively to have carried out comparative example 25-28 with the same way of embodiment 1-4, the described Chinese fiber crops bast fiber extract called after D25-28 successively obtained.
Active testing
For examination bacterial classification
This experimental technique staphylococcus aureus (Staphylococcusaureus used, CMCC (B) 26003), pseudomonas aeruginosa (Pseudomonasaeruginosa, and Candida albicans (Candidasalbicans ATCC27835), CMCC (F) 98001), be all purchased from Huan Kai bio tech ltd, Guangdong, Guangzhou.
Bacteriostatic test
1, staphylococcus aureus, pseudomonas aeruginosa are activated with the nutrient agar be available commercially respectively, by the Candida albicans potato dextrose agar activation be available commercially.
Bacterium liquid sterile saline after activation is diluted to 10
7cFU/mL, the nutrient agar be then available commercially with 100mL mixes, and shakes up, and obtained concentration is 10
5the bacterium liquid culture medium of CFU/mL.
2, test sample prepares: Chinese fiber crops bast fiber extract volumetric concentration the present invention obtained is dimethyl sulfoxide (DMSO) (DMSO) aqueous dissolution of 20%, be mixed with the solution that mass body volume concentrations is 10mg/mL, add Tween 80 and carry out hydrotropy, the addition of Tween 80 should be less than 10% of gained system cumulative volume after hydrotropy.
3, Odontothrips loti measures antibacterial circle diameter: after the nutrient agar be available commercially melts, get 10 milliliters in culture dish, after its cooled and solidified, get bacterium liquid culture medium in 5 milliliters of above-mentioned steps 1 in culture dish, jiggle, make it be evenly distributed in planar surface, treat that it cools, flat board is put into Oxford cup, adds the 200 μ L test samples obtained in step 2 respectively.
Staphylococcus aureus, pseudomonas aeruginosa are measured antibacterial circle diameter after cultivating 24 hours at 37 DEG C, and Candida albicans is measured and records measurement inhibition zone size for 4 days afterwards by right-angled intersection method 28 DEG C of cultivations.Volumetric concentration is adopted to be the DMSO aqueous solution of 20% and mixed solution (both volume ratios the are 1:1) sample in contrast of Tween 80, every ware 4 Oxford cups (Oxford cup diameter 8mm) are equidistantly placed, every bacterium three Duplicate Samples, control sample measures inhibition zone size after adopting identical cultural method, result gets the mean value of three tests, obtain the Chinese of the present invention fiber crops bast fiber extract to the fungistatic effect of different strains tested, judge bacteriostasis by inhibition zone size.More than operate and all aseptically carry out.
Results and analysis
Bacteriostasis result is as shown in table 2 below:
Table 2
Note: " * " wherein represents that the antibacterial circle diameter of all control groups is all less than 8.00mm.
From upper table 2, Chinese fiber crops bast fiber extract of the present invention all has antibacterial action in various degree to 3 kinds of strains testeds, and it is the strongest to the antibacterial action of staphylococcus aureus, and being secondly pseudomonas aeruginosa, is finally Candida albicans.
In addition, it can also be seen that from table 2, only have the specific extraction solvent adopted in the inventive method, the dissolving of saturated aqueous common salt, the dress post of swelling silica gel and compound eluting solvent, just can obtain best active component to extract, such as in the leaching process of step (3), only have and adopt ethanol just can obtain best effect, and when using methyl alcohol, normal propyl alcohol, n-butanol, fungistatic effect all there is remarkable reduction.On the other hand, when adding the acetone of special ratios further in the bi-component eluting solvent of chloroform, methyl alcohol, further improve the bactericidal effect of extract, prove that adding of acetone significantly improves extraction effect, there is excellent collaborative composite soil washing.
In sum, the present inventor has paid a large amount of creative works and has developed a kind of Chinese fiber crops bast fiber extract, extracting method and the purposes with antibacterial activity, by the selection adopting the liquid-liquid extraction of Solvent Extract methods, mineral solution and organic solvent, specific silica gel fills post and specific eluting solvent, and achieve good extraction effect, extract obtained have good killing and inhibitory action to various bacteria.And when adding acetone further in eluting solvent system, find to further increase extraction effect.Extract of the present invention, extracting method and purposes industrially have good research, using value, have wide application potential and prospect simultaneously.
Should be appreciated that the purposes of these embodiments is only not intended to for illustration of the present invention limit the scope of the invention.In addition; also should understand; after having read technology contents of the present invention, those skilled in the art can make various change, amendment and/or modification to the present invention, and these all equivalent form of values fall within the protection domain that the application's appended claims limits equally.
Claims (5)
1. a preparation method for Chinese fiber crops bast fiber extract, described method comprises the steps:
(1) raw material is washed;
(2) dry, shred;
(3) Solvent Extract methods;
(4) reduced pressure concentration, obtains primary extract medicinal extract;
(5) primary extract medicinal extract is carried out the liquid-liquid extraction using mineral solution and organic solvent, obtain medicinal extract;
(6) medicinal extract is loaded in silica gel column chromatography, organic solvent wash-out, collect eluent, reduced pressure concentration, obtain described Chinese fiber crops bast fiber extract;
Described step (5) concrete operations are as follows: fully shaken up by the saturated NaCl aqueous solution of primary extract medicinal extract, dissolve, suction filtration, obtain aqueous phase and non-dissolved solid; Non-dissolved solid ethyl acetate is fully shaken up, dissolves, obtains ethyl acetate phase; Described aqueous phase and ethyl acetate are added in separatory funnel, fully shake up, mix, stratification, aqueous phase discarded, by ethyl acetate phase reduced pressure concentration, obtain ethyl acetate phase medicinal extract;
Described step (6) concrete operations are as follows: fully dissolved by ethyl acetate phase medicinal extract chloroform, and to join granularity be in 200-300 object silica gel, stir, obtain silica gel absorption sample; Described silica gel absorption sample is joined the silica gel column chromatography top filled, then mixed organic solvents is used to carry out wash-out, started to collect elute soln by time bottom solvent washing to chromatographic column until sample, collect the elute soln being equivalent to 2-4 column volume, by this elute soln reduced pressure concentration, obtain described Chinese fiber crops bast fiber extract;
Described silica gel column chromatography fills post as follows: be soaked in chloroform by 200-300 object silica gel, and fully swelling, till no longer swelling, then fills post, and sedimentation one is late;
The described organic solvent carrying out wash-out is the mixture of chloroform, methyl alcohol and acetone, and wherein the volume ratio of chloroform, methyl alcohol, acetone is 46-50:1:2-4.
2. preparation method as claimed in claim 1, is characterized in that: the organic solvent in described step (3) is the lower alcohol with 1-6 carbon atom.
3. preparation method as claimed in claim 1 or 2, is characterized in that: the described organic solvent carrying out wash-out is the mixture of chloroform, methyl alcohol and acetone, and wherein the volume ratio of chloroform, methyl alcohol, acetone is 46-50:1:3.
4. the Chinese fiber crops bast fiber extract for preparing of method according to claim 1.
5. the purposes of described Chinese fiber crops bast fiber extract as claimed in claim 4 in textile field.
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| CN105124607A (en) * | 2015-07-28 | 2015-12-09 | 桐城市牯牛背农业开发有限公司 | Extraction process for cress fiber |
| CN105455147A (en) * | 2015-11-18 | 2016-04-06 | 桐城市牯牛背农业开发有限公司 | A lepidium sativum fiber extracting process |
| CN108103589A (en) * | 2018-01-24 | 2018-06-01 | 辽宁轻工职业学院 | A kind of apocynum bast fiber supercritical carbon dioxide degumming and antibiotic finish system |
| CN109161578A (en) * | 2018-08-20 | 2019-01-08 | 广西巴马常春藤生命科技发展有限公司 | A kind of environment-friendly function detection method of hemp stalk core fibre film |
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| CN1742736A (en) * | 2005-08-16 | 2006-03-08 | 水利部沙棘开发管理中心 | Buckthorn extract, its preparing method and use in pharmaceutical process |
| CN101028341A (en) * | 2007-02-13 | 2007-09-05 | 韩颖 | Magnoliaceae plant extract, its production and use |
| CN102648716A (en) * | 2012-03-27 | 2012-08-29 | 江苏紫荆花纺织科技股份有限公司 | Extraction method and purpose of jute fiber extracts with bacteriostatic activity |
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| CN1742736A (en) * | 2005-08-16 | 2006-03-08 | 水利部沙棘开发管理中心 | Buckthorn extract, its preparing method and use in pharmaceutical process |
| CN101028341A (en) * | 2007-02-13 | 2007-09-05 | 韩颖 | Magnoliaceae plant extract, its production and use |
| CN102648716A (en) * | 2012-03-27 | 2012-08-29 | 江苏紫荆花纺织科技股份有限公司 | Extraction method and purpose of jute fiber extracts with bacteriostatic activity |
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| 狭叶荨麻叶中荨麻皂苷的提取与鉴定研究;张海悦等;《食品科学》;20081231;第29卷(第11期);第282-283页 * |
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| WO2023172982A3 (en) * | 2022-03-08 | 2023-11-09 | Trade Secret Chocolates | Systems and methods for rehabilitating alcohol compositions and naturally fermentable herbs |
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