CN101828750B - Method for extracting natural preservative from bamboo leaves - Google Patents
Method for extracting natural preservative from bamboo leaves Download PDFInfo
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- CN101828750B CN101828750B CN201010175102A CN201010175102A CN101828750B CN 101828750 B CN101828750 B CN 101828750B CN 201010175102 A CN201010175102 A CN 201010175102A CN 201010175102 A CN201010175102 A CN 201010175102A CN 101828750 B CN101828750 B CN 101828750B
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- 235000017166 Bambusa arundinacea Nutrition 0.000 title claims abstract description 87
- 235000017491 Bambusa tulda Nutrition 0.000 title claims abstract description 87
- 241001330002 Bambuseae Species 0.000 title claims abstract description 87
- 235000015334 Phyllostachys viridis Nutrition 0.000 title claims abstract description 87
- 239000011425 bamboo Substances 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 51
- 239000003755 preservative agent Substances 0.000 title abstract description 11
- 230000002335 preservative effect Effects 0.000 title abstract description 9
- 238000000605 extraction Methods 0.000 claims abstract description 65
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- -1 feed Substances 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 35
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- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 description 4
- 150000007965 phenolic acids Chemical class 0.000 description 4
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 description 4
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- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
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- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
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- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
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- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- 240000002014 Phyllostachys nigra var. henonis Species 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
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- Cosmetics (AREA)
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention provides a method for extracting and preparing a natural, safe and high-efficiency plant natural preservative by using bamboo leaves as raw materials and integrating an ultrasonic auxiliary extraction technology, a membrane separation technology, a composite solvent continuous countercurrent extraction technology, a vacuum concentration technology, and the like. The preservative can be widely applied to fruits, vegetables, food, medicines, feed, cosmetics, and the like, and particularly, the preservative has broad antibacterial spectrum and small additive amount and belongs to clarification type preservatives in beverages. After the preservative is added to beverage products, the preservative cannot influence the color, the flavor and the taste of the products, thus the preservative has obvious application advantages.
Description
Technical field
The present invention relates to a kind of method of from the leaf of bamboo, extracting natural antiseptic agent; Relate in particular to a kind of integrated ultrasonic auxiliary extraction technology, membrane separation technique, double solvents continuous countercurrent extraction technology, and vacuum concentration technique etc. is extracted the method for the active natural antiseptic agent of the leaf of bamboo.
Background technology
Not having food preservative is an inconceivable thing.Use 100,000 tons of chemical synthesis anticorrisive agents year with present China, on average calculate, make every year 100000000 tons of food not putrid and deteriorated by 1 ‰ additive capacities.Average food per ton is by 3000 yuan of calculating, and direct economy is worth and reaches 3,000 hundred million yuan! It is thus clear that food industry at present is to be unable to do without food preservative, developed country is no exception.
In view of of the threat of chemical synthesis food preservative to health; The additive capacity of this based food anticorrisive agent of the strict control in each national capital; Even so; Progressive along with technologically, scientists is found the accumulation property chronic injury that the chemical synthesis food preservative causes human body more and more, and these injuries overwhelming majority is irreversible.In this case, many countries examine the use to the chemical synthesis food preservative again closely, and country with good conditionsi has begun to completely forbid the partly use of chemical food preservative.Having completely forbidden the highest chemical synthesis food preservative Sodium Benzoate of toxicity like Japan uses in fruits and vegetables, food, medicine, feed and cosmetics.China also forbids adding Sodium Benzoate in numerous food product.Last March, FSA is March 2 2006 local time, and at its official website title that publishes the news, some soft drinks possibly produce carcinogenic substance benzene.This office is thought, receives and these two kinds of compositions of vitamin C (anti-oxidant) if carbonated drink is contained chemical synthesis food preservative benzoic acid simultaneously, and possibly produce interacts generates benzene; And benzene is high carcinogenic substance.Comprise numerous popular soft drinks such as Finda carbonated drink, Mirinda orange juice, all contain chemical synthesis preservative sodium benzoate and anti-oxidant, possibly constitute carcinogenic danger.
In the world, food additives are to natural, nutrition and the development of functionalization aspect, and research is extensive day by day with application, but still belong to the primary stage in China.In recent years, because many antiseptics for natural food have been developed in the R&D institution of China and the positive effort of production unit, wherein many kinds are being widelyd popularize and are being used and obtaining gratifying effect.Development along with food industry; The raising of people's living standard and awareness of safety; Security to some synthetic preservatives is constantly queried, and the scientific worker holds prudent scientism to the chemical synthesis anticorrisive agent, and the consumer then abstains from the non-natural food preservative very much.Given this, seek safety, antiseptics for natural food becomes the research focus of food industry efficiently.Consider that from security, resource and economy exploitation vegetable source natural food preservative becomes first-selection in China.
The leaf of bamboo is the leaf of grass henon bamboo, with characteristics such as its unique biological, ecology and multipurposes, receives people's attention day by day.It is reported that bamboo extractive active ingredient contains flavonoids and the compounds relevant with the human life activity such as glycoside, active polysaccharide class, extraordinary amino acid and derivative thereof thereof; Contain multiple element that can activating human body cells such as manganese, zinc, selenium, germanium, silicon, and be master's fragrance ingredient etc. with aldehyde, alcohol.The extract of the leaf of bamboo has good Green Tea Extract, anti-oxidant, anti-ageing, antifatigue, reducing blood lipid, prevention cardiovascular and cerebrovascular disease and protection liver, anticancer disease, beautify effect such as skin.
In recent years, people have carried out number of research projects around the analysis and the extract thereof of bamboo class main chemical compositions.Wherein maximum is relevant research of from the leaf of bamboo, extracting flavone compound.For example; Chinese patent 98104564.2 discloses a kind of production method of from the leaf of bamboo, extracting flavonoid compound extract or pulvis; With the leaf of bamboo is raw material, and through extraction, concentrated, separation, refining or dry again, obtaining with the bamboo-leaves flavones glucosides is master's flavone compound.But its technology also rests on the chamber stage, needs to consume a large amount of organic solvents, and preparation cost is high, and is easy to generate environmental pollution.
(summarize in the progress of experiment and theoretical side domestic and international bamboo extractive by " living beings Chemical Engineering " (2008, vol42, No.3)) in " active ingredient of bamboo extractive and Research development thereof " for He Yuejun etc.Introduce the active ingredient of bamboo extractive respectively, comprised the extraction and the isolation technics of flavone compound, polysaccharide, mineral element and other compositions.
But; Adopt complete extraction process continuously; Effective active composition to contained in the leaf of bamboo comprises flavone compound, phenolic acid compound, bioactive polysaccharide etc., extracts continuously; And obtain the research of natural compound (containing flavone compound, phenolic acid compound, bioactive polysaccharide etc.) anticorrisive agent, at home and abroad do not appear in the newspapers at present.
Summary of the invention
The object of the present invention is to provide a kind of integrated ultrasonic auxiliary extraction technology, membrane separation technique, double solvents continuous countercurrent extraction technology; And vacuum concentration technique; To effective active composition contained in the leaf of bamboo; Comprise flavone compound, phenolic acid compound, bioactive polysaccharide etc., extract continuously, and obtain the method for the active natural antiseptic agent of pure natural compound (containing flavone compound, phenolic acid compound, bioactive polysaccharide etc.).
The objective of the invention is to be realized by following technical scheme: a kind of method of from the leaf of bamboo, extracting natural antiseptic agent may further comprise the steps:
1) with for use after the fresh leaf of bamboo collection clean dry;
2) leaf of bamboo is put into extractor; Add the ethanol of volume fraction 60%, solid-to-liquid ratio 1: 7-1: 10 (mL/g) are heated to 40 ℃-80 ℃; It with the frequency auxiliary 0.5-1 hour of the ultrasonic wave of 50-150KHz; Lixiviate 0.5-2.5 hour then, the active ingredient in the leaf of bamboo fully is dissolved in the ethanolic solution, leach solution for later use;
3) with above-mentioned solution through the secondary filter device, remove large granular impurity, clear filtrate;
4) with above-mentioned filtrating through the tubular type nanofiltration membrane treatment, obtain seeing through liquid and trapped fluid, wherein to see through liquid concentrated through reducing pressure, the ethanol that obtains reclaiming;
5) the trapped fluid process rolling ultrafiltration membrane treatment that step 4 is obtained obtains seeing through liquid and trapped fluid, and the liquid that sees through is wherein made health products through post processing;
That 6) adopts trapped fluid that double solvents obtains step 5 carries out the continuous centrifugal counter-current extraction, obtains some extraction phases respectively;
7) the said some extraction phases that step 6 obtained concentrate through film and obtain leaf of bamboo extraction natural antiseptic agent.
In the plant extract process, leaching process is first key problem in technology of the present invention.According to the record of the document of prior art, and inventor's experimental result repeatedly, in said leaching process, the lixiviate solid-liquid ratio, solvent and concentration thereof, extraction temperature, the time etc. are again the keys in the leaching process.
In order to obtain the natural antiseptic agent that from the leaf of bamboo, extracts of the present invention, the leaf of bamboo of the present invention compares 1 with the liquid material of solvent: 7-1: 10 (mL/g, down together), and preferred solid-liquid ratio is 1: 10; The inventor adopts ethanol water as extracting solvent, and its concentration range is at 40%-80% (percentage by volume, down together), the preferably ethanol water of 60% concentration; Extraction temperature is at 40 ℃-80 ℃, and preferred extraction temperature is 60 ℃; Extraction time is at 0.5-2.5 hour, preferred extraction time 1-2 hour.Simultaneously, in order to obtain the effective active components in the leaf of bamboo to greatest extent, the present invention adopts ultrasonic wave to assist the ethanol lixiviate, and ultrasonic treatment time is at 0.5-1 hour, preferred time 0.5-0.75 hour; The ultrasonic Treatment frequency is at 50-150KHZ, and the preferred process frequency is at 80-100KHZ.
As preferably, secondary filter device according to the invention can be ceramic membrane, millipore filter, cloth envelop collector, filtering accuracy 0.5 μ m-10 μ m, preferred 0.5 μ m-1 μ m.
According to a kind of method of from the leaf of bamboo, extracting natural antiseptic agent of the present invention, concentrated, the separation process of leaching liquor are second key problem in technology.
According to the present invention, at first adopt NF membrane to concentrate, separate to ethanol lixiviate bamboo extractive.Can be used to reclaim ethanol on the one hand, the ethanol rate of recovery can reach more than 90%; Can concentrate leaching liquor on the other hand, simultaneously reduce operating temperature greatly, prevent that thermally sensitive composition Yin Wendu in the leaf of bamboo active matter is too high and destroy.
In the organic facies system, it is a new research field that the applying nano filtering technique separates.Obtained application more and more widely in recent years.But most NF membrane can only be applied to the water system, if be applied to organic solvent system, they will lose integrality and original separating property of structure.Thereby the unstability of film can cause the expansion of film or breaking of film to obtain very large membrane flux on the one hand.Thereby the contraction that can also cause film on the other hand makes solvent can not see through film.Therefore, NF membrane in organic solvent unstability and in organic facies the Determination of Parameters that influences of nanofiltration transport mechanism be anxious major issue to be solved.
The inventor has investigated the influence to the organic solvent membrane flux of pressure, temperature and feed liquid flow velocity, thereby confirms to influence in the organic system parameter of membrane flux.On this basis, expectation utilizes these parameters to set up the flux TRANSFER MODEL of NF membrane in organic solvent.Confirm that the optimum process condition that this project adopts nanofiltration to reclaim alcohol solvent is: adopt 2.5 inches tubular type nanofiltration membrane component systems of polyamide material, operating temperature is below 30 ℃, pressure 0.5～1.0Mpa, operating flux 0.15～0.30m3/h.
According to the present invention the nanofiltration of leaching liquor concentrate, separation process, the NF membrane molecular cut off is at 200-500Da, and the rate of recovery of ethanol is reached more than 95, concentrates extract solution of bamboo leaves more than 60 times simultaneously.
Through the extract solution of bamboo leaves of nanofiltration once concentration, continue to utilize the back pressure of nanofiltration system, send into milipore filter and carry out secondary concentration, separation; Concentration rate is more than 30 times; Thus can be further effective ingredient in the enrichment leaf of bamboo effectively, improve content of effective, extract yield and improve 6%.
The inventor adopts the rolling milipore filter of molecular cut off in the polysulfones material (PS) of 4000-6000Da, and it is high that rolling milipore filter film core is loaded density, and elementary membrane area cost is low; Operating pressure is lower, can satisfy the concentrated refinement treatment technological requirement of this project extract solution of bamboo leaves fully.
Therefore; The inventor makes full use of concentrated, the stalling characteristic function of membrane separation technique; Development and Design the membrane technology integrated technique; Reduction, enrichment and extract effective active components contained in the leaf of bamboo effectively, the solvent that also can farthest use the technology pilot process simultaneously recycled, and realizes the doulbe-sides' victory of economic benefit and environmental protection and energy saving.
According to a kind of method of from the leaf of bamboo, extracting natural antiseptic agent of the present invention, extraction process is the 3rd key problem in technology.In order to obtain the effective active components in the leaf of bamboo to greatest extent, and obtain the natural antiseptic agent that from the leaf of bamboo, extracts of the present invention.The inventor adopts centrifugal extracter continuous countercurrent extraction system, adopts the double solvents of some kinds of opposed polarities to carry out fractional extraction to the bamboo extractive aqueous solution, obtains some different extraction phases.Feed liquid is the extract after film separates, and adopts continuous countercurrent extracting operation, and optimum parameters comprises: the volume ratio of counter-current extraction progression, feed liquid and solvent etc.
Centrifugal extractor is widely used in liquid/liquid extraction or the separation field that does not conform to solid or contain the small amount of solid system; Multi-stage counter current extraction technology is suitable for the operating procedure of double solvents continuous countercurrent extraction bamboo extractive; Its advantage is to make each extracting stage all to obtain bigger mass transfer force; Leaf of bamboo effective component extraction rate is high, and the unit volume extractant rises to the entrainment of leaf of bamboo active ingredient, has reduced the solvent use amount.Counter-current extraction progression is very remarkable to the influence of leaf of bamboo effective component extraction rate, and recovery rate increases along with the increase of extraction progression, but behind the multi-stage counter current extraction, the leaf of bamboo effective component extraction rate value of tending towards stability.As a whole; The continuous countercurrent extraction method has than two much higher alternate concentration differences of batch method extraction; Also can obtain enough recovery rates thereby increased the mass transfer driving force at the less extractant of use with under, thereby reduce the liquid waste processing amount and save production cost than the situation of skinny device.
According to extraction process of the present invention, counter-current extraction progression is 2 to 4 grades, preferred 3 grades.Said extractant can be selected from a kind of or its mixture of ethyl acetate, carrene, n-butanol, chloroform, benzinum, ethyl acetate, acetone.
As preferably, the operating parameter of continuous countercurrent extracting operation process according to the invention is: the extraction of three stage countercurrents, extractant: the ratio of trapped fluid is 1: 1 to 1: 5.With batch extraction phase ratio, continuous countercurrent extraction has reduced the consumption of extractant, is 2/3 of traditional extraction agent (ethyl acetate) consumption, and extraction yield reaches 93%, extracts yield and improves 6% than traditional method.
According to Centrifugical extraction process of the present invention, the rotating speed of centrifugal extractor is 1500rpm-3000rpm, and preferred rotating speed is 2000rpm-2500rpm.
According to a kind of method of from the leaf of bamboo, extracting natural antiseptic agent of the present invention, comprise that also said some extraction phases concentrate the process that the leaf of bamboo extracts natural antiseptic agent that obtains through film.As preferably, the process conditions that film concentrates are: 40 ℃-70 ℃ of temperature; Vacuum 0.07Mpa-0.09Mpa.
Adopt filter paper method, dilution plate counting method; Measure the bacteriostatic activity of the different extraction parts of bamboo extractive; The result shows: a kind of natural antiseptic agent that from the leaf of bamboo, extracts of the present invention has the anti-corrosive antibacterial effect, to the staphylococcus aureus killing rate greater than 90%, to the Escherichia coli killing rate greater than 90%, to the bacillus subtilis killing rate greater than 90%.
Therefore, the invention has the beneficial effects as follows:
1, with the leaf of bamboo is raw material; Extraction has the leaf of bamboo active matter of antiseptic and inhibiting bacteria function effect; And its preparation technology optimized; A kind of pure natural, safety, the natural antiseptic agent of plant leaf of bamboo extraction have efficiently been made; Its effective active components comprises at least: polysaccharide (in total reducing sugar): 2%-10%, phenolic acid: 0.2%-1.0%, general flavone (in rutin): 0.5%-2.0%, the compound preservative of the pure natural that is extracted to the staphylococcus aureus killing rate greater than 90%, to the Escherichia coli killing rate greater than 90%, to the bacillus subtilis killing rate greater than 90%.
2, integrated ultrasonic auxiliary acid alcohol extract technology, double solvents continuous countercurrent extraction technology, membrane separation technique, film concentration technique and fluidized drying technology etc.; Development and Design continuous complete extraction process; To effective active composition contained in the leaf of bamboo, comprise that flavone compound, phenolic acid compound, bioactive polysaccharide etc. extract continuously, and the anti-corrosive antibacterial effect that has of acquisition pure natural is extracted natural antiseptic agent; Extraction efficiency is high, and cost is low.
The specific embodiment
Through embodiment, do further bright specifically below to technical scheme of the present invention.But it can not be interpreted as it is limitation of the present invention.
Embodiment 1
By technological process shown in Figure 1, from the leaf of bamboo, extract the method for natural antiseptic agent, may further comprise the steps:
1) with for use after the fresh leaf of bamboo collection clean dry;
2) the 300kg leaf of bamboo is put into extractor, add the ethanol of 30000ml volume fraction 60%, be heated to 60 ℃; It with the frequency auxiliary 0.5 hour of the ultrasonic wave of 50KHz; Lixiviate is 1.5 hours then, and the active ingredient in the leaf of bamboo fully is dissolved in the ethanolic solution, leaches solution for later use;
3) with the microporous filter of above-mentioned solution, remove large granular impurity, get clear filtrate through filtering accuracy 0.5 μ m;
4) with the 2.5 inch tubular type nanofiltration membrane component system handles of above-mentioned filtrating through the polyamide material, its molecular cut off 300Da, operating temperature is below 30 ℃, and pressure keeps 0.5Mpa, and operating flux remains on 0.25m3/h.Obtain seeing through liquid and trapped fluid, wherein to see through liquid concentrated through reducing pressure, the ethanol that obtains reclaiming;
5) trapped fluid that step 4 is obtained passes through the rolling ultrafiltration membrane treatment of polysulfones material (PS), its molecular cut off 5000Da, and operating temperature is below 30 ℃; Pressure keeps 0.15Mpa; Operating flux remains on 0.2m3/h, obtains seeing through liquid and trapped fluid, and the liquid that sees through is wherein made health products through post processing;
6) adopt the three grades of continuous centrifugal counter-current extractions that carry out of trapped fluid that double solvents obtains step 5; Adopt ethyl acetate, carrene, n-butanol as extractant respectively; Extractant: the ratio of trapped fluid is 1: 5, and centrifugal rotational speed 1500rpm obtains some extraction phases respectively;
7) the said some extraction phases that step 6 obtained concentrate through film, 50 ℃ of control temperature, and vacuum 0.07Mpa obtains the leaf of bamboo and extracts natural antiseptic agent.
Adopt AAS that the extract leaf of bamboo that obtains is extracted natural antiseptic agent and analyze, its effective active components comprises at least: polysaccharide (in total reducing sugar): 6.3%; , phenolic acid: general flavone (in rutin) 0.67%: 1.85%.
Embodiment 2
By technological process shown in Figure 1, from the leaf of bamboo, extract the method for natural antiseptic agent, may further comprise the steps:
1) with for use after the fresh leaf of bamboo collection clean dry;
2) the 300kg leaf of bamboo is put into extractor, add the ethanol of 21000ml volume fraction 60%, be heated to 60 ℃; It with the frequency auxiliary 0.75 hour of the ultrasonic wave of 100KHz; Lixiviate is 2.0 hours then, and the active ingredient in the leaf of bamboo fully is dissolved in the ethanolic solution, leaches solution for later use;
3) with the microporous filter of above-mentioned solution, remove large granular impurity, get clear filtrate through filtering accuracy 0.5 μ m;
4) with the 2.5 inch tubular type nanofiltration membrane component system handles of above-mentioned filtrating through the polyamide material, its molecular cut off 400Da, operating temperature is below 30 ℃, and pressure keeps 0.75Mpa, and operating flux remains on 0.3m3/h.Obtain seeing through liquid and trapped fluid, wherein to see through liquid concentrated through reducing pressure, the ethanol that obtains reclaiming;
5) trapped fluid that step 4 is obtained passes through the rolling ultrafiltration membrane treatment of polysulfones material (PS), its molecular cut off 4000Da, and operating temperature is below 30 ℃; Pressure keeps 0.10Mpa; Operating flux remains on 0.25m3/h, obtains seeing through liquid and trapped fluid, and the liquid that sees through is wherein made health products through post processing;
6) adopt the three grades of continuous centrifugal counter-current extractions that carry out of trapped fluid that double solvents obtains step 5; Adopt ethyl acetate, carrene, n-butanol as extractant respectively; Extractant: the ratio of trapped fluid is 1: 5, and centrifugal rotational speed 2000rpm obtains some extraction phases respectively;
7) the said some extraction phases that step 6 obtained concentrate through film, 60 ℃ of control temperature, and vacuum 0.08Mpa obtains the leaf of bamboo and extracts natural antiseptic agent.
Adopt AAS that the extract leaf of bamboo that obtains is extracted natural antiseptic agent and analyze, its effective active components comprises at least: polysaccharide (in total reducing sugar): 7.2%; , phenolic acid: general flavone (in rutin) 0.77%: 1.95%.
Embodiment 3
By technological process shown in Figure 1, from the leaf of bamboo, extract the method for natural antiseptic agent, may further comprise the steps:
1) with for use after the fresh leaf of bamboo collection clean dry;
2) the 300kg leaf of bamboo is put into extractor, add the ethanol of 24000ml volume fraction 60%, be heated to 60 ℃; It with the frequency auxiliary 1 hour of the ultrasonic wave of 120KHz; Lixiviate is 0.75 hour then, and the active ingredient in the leaf of bamboo fully is dissolved in the ethanolic solution, leaches solution for later use;
3) with the microporous filter of above-mentioned solution, remove large granular impurity, get clear filtrate through filtering accuracy 0.5 μ m;
4) with the 2.5 inch tubular type nanofiltration membrane component system handles of above-mentioned filtrating through the polyamide material, its molecular cut off 500Da, operating temperature is below 30 ℃, and pressure keeps 0.75Mpa, and operating flux remains on 0.3m3/h.Obtain seeing through liquid and trapped fluid, wherein to see through liquid concentrated through reducing pressure, the ethanol that obtains reclaiming;
5) trapped fluid that step 4 is obtained passes through the rolling ultrafiltration membrane treatment of polysulfones material (PS), its molecular cut off 6000Da, and operating temperature is below 30 ℃; Pressure keeps 0.10Mpa; Operating flux remains on 0.25m3/h, obtains seeing through liquid and trapped fluid, and the liquid that sees through is wherein made health products through post processing;
6) adopt the three grades of continuous centrifugal counter-current extractions that carry out of trapped fluid that double solvents obtains step 5; Adopt ethyl acetate, carrene, n-butanol as extractant respectively; Extractant: the ratio of trapped fluid is 1: 3, and centrifugal rotational speed 2500rpm obtains some extraction phases respectively;
7) the said some extraction phases that step 6 obtained concentrate through film, 60 ℃ of control temperature, and vacuum 0.09Mpa obtains the leaf of bamboo and extracts natural antiseptic agent.
Adopt complexing-AAS that the extract leaf of bamboo that obtains is extracted natural antiseptic agent and analyze, its effective active components comprises at least: polysaccharide (in total reducing sugar): phenolic acid 8.1%: general flavone (in rutin) 0.83%: 1.79%.
Comparative Examples
1) with for use after the fresh leaf of bamboo collection clean dry;
2) the 300kg leaf of bamboo is put into extractor, add the ethanol of 24000ml volume fraction 60%, be heated to 60 ℃, lixiviate 2.5 hours fully is dissolved in the ethanolic solution active ingredient in the leaf of bamboo, leaches solution for later use;
3) with the microporous filter of above-mentioned solution, remove large granular impurity, get clear filtrate through filtering accuracy 0.5 μ m;
4) above-mentioned feed liquid is handled through tubular ultra-filtration membrane; Obtain seeing through liquid and trapped fluid, trapped fluid wherein concentrates through decompression, in spray tower, is spray dried to powdery again; 160 ℃ of control EATs; 87 ℃ of leaving air temps obtain general flavone content and are 15.5% bamboo-leaves flavones product, additive capable of using as feed;
5) an above-mentioned part that sees through the liquid people is concentrated through decompression, in spray tower, be spray dried to powdery again, 165 ℃ of control EATs, 90 ℃ of leaving air temps:, obtain general flavone content and be 25.8% bamboo-leaves flavones product, can make the health food raw material;
6) an above-mentioned part that sees through liquid is put into the intermediate treatment jar, adding HC1 regulator solution acid-base value to pH value is 4.2, through the rolling ultrafiltration membrane treatment; Obtain seeing through liquid and trapped fluid; The liquid that sees through wherein concentrates through the processing of sodium filter membrane, and the low molecule flavonoids of part, aldehydes matter and glucide are concentrated through reducing pressure by the sodium membrane retention again; It is 4.6% bamboo-leaves flavones medicinal extract product that instantaneous sterilizing obtains general flavone content, and the bamboo extractive that can make the liquid food nutrition fortifier concentrates refined juice;
7) part with above-mentioned trapped fluid concentrates through decompression, in spray tower, is spray dried to powdery again, 170 ℃ of control EATs, and 92 ℃ of leaving air temps, obtaining general flavone content is 31.5% bamboo-leaves flavones product, can make food additives;
8) adopt macroporous absorbent resin to adsorb a dissection process part of above-mentioned trapped fluid, eluent is concentrated after microwave drying obtains general flavone content is 51.5% bamboo-leaves flavones product, can make medicine intermediate or cosmetic material.
Experimental example
Adopt filter paper method, dilution plate counting method, measure the bacteriostatic activity that the leaf of bamboo that is obtained in the foregoing description 1-3 and the Comparative Examples extracts natural antiseptic agent, the result is like table 1, shown in 2
Table 1 extract inhibition zone size
Table 2 extract fungistatic effect
Show: the natural antiseptic agent that from the leaf of bamboo, extracts of the present invention with respect to the bamboo extractive that prior art processes obtained, has obviously good bacteriostatic activity effect.
Claims (8)
1. method of from the leaf of bamboo, extracting natural antiseptic agent is characterized in that said method comprising the steps of:
1) with for use after the fresh leaf of bamboo collection clean dry;
2) leaf of bamboo is put into extractor; Add the ethanol of volume fraction 60%, solid-to-liquid ratio 1: 7-1: 10 (mL/g) are heated to 40 ℃-80 ℃; It with the frequency auxiliary 0.5-1 hour of the ultrasonic wave of 50-150KHz; Lixiviate 0.5-2.5 hour then, the active ingredient in the leaf of bamboo fully is dissolved in the ethanolic solution, leach solution for later use;
3) with above-mentioned solution through the secondary filter device, remove large granular impurity, clear filtrate;
4) with above-mentioned filtrating through the tubular type nanofiltration membrane treatment, obtain seeing through liquid and trapped fluid, wherein to see through liquid concentrated through reducing pressure, the ethanol that obtains reclaiming;
5) the trapped fluid process rolling ultrafiltration membrane treatment that step 4 is obtained obtains seeing through liquid and trapped fluid, and the liquid that sees through is wherein made health products through post processing;
6) adopt double solvents that the trapped fluid that step 5 obtains is carried out the continuous centrifugal counter-current extraction, obtain some extraction phases respectively;
7) the said some extraction phases that step 6 obtained concentrate through film and obtain leaf of bamboo extraction natural antiseptic agent.
2. a kind of method of from the leaf of bamboo, extracting natural antiseptic agent according to claim 1 is characterized in that:
Said secondary filter device is ceramic membrane, millipore filter or cloth envelop collector, filtering accuracy 0.5 μ m-10 μ m.
3. a kind of method of from the leaf of bamboo, extracting natural antiseptic agent according to claim 1 is characterized in that:
Said NF membrane adopts 2.5 inches tubular type nanofiltration membrane component systems of polyamide material, and the control operation temperature is below 30 ℃, pressure 0.5～1.0Mpa, operating flux 0.15～0.30m
3/ h.
4. a kind of method of from the leaf of bamboo, extracting natural antiseptic agent according to claim 1 is characterized in that:
Said milipore filter adopts the rolling milipore filter of molecular cut off at the polysulfones material PS of 4000-6000Da.
5. a kind of method of from the leaf of bamboo, extracting natural antiseptic agent according to claim 1 is characterized in that:
Said continuous centrifugal counter-current extraction process, counter-current extraction progression are 2 to 4 grades, and trapped fluid is 1 with the ratio of extractant: 1-1: 5.
6. a kind of method of from the leaf of bamboo, extracting natural antiseptic agent according to claim 5 is characterized in that:
Said extractant is selected from a kind of or its mixture of ethyl acetate, carrene, n-butanol, chloroform, benzinum, acetone.
7. a kind of method of from the leaf of bamboo, extracting natural antiseptic agent according to claim 1 is characterized in that;
The centrifugal rotational speed of said Centrifugical extraction process is 1500rpm-3000rpm.
8. according to each described a kind of method of from the leaf of bamboo, extracting natural antiseptic agent among the claim 1-7, it is characterized in that; The process conditions that said film concentrates are: 40 ℃-70 ℃ of temperature; Vacuum 0.07Mpa-0.09Mpa.
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| CN104938544A (en) * | 2015-06-24 | 2015-09-30 | 陈琳仁 | Method for preparing natural preservative and application thereof |
| CN105687826A (en) * | 2016-01-29 | 2016-06-22 | 上海海中实业有限公司 | Bamboo leaf extract as well as preparation method and application thereof |
| CN108014038A (en) * | 2016-11-04 | 2018-05-11 | 无锡法瑞雅生物细胞科学有限公司 | A kind of skin-moisturizing, skin water and preparation method thereof |
| CN108770917A (en) * | 2018-04-20 | 2018-11-09 | 浙江省海洋水产研究所 | A kind of dry preservative of krill and preparation method thereof, application |
| CN115372519A (en) * | 2022-09-21 | 2022-11-22 | 广西壮族自治区水牛研究所 | Gas chromatography detection method for ethanol in silage |
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