(3) summary of the invention
The object of the invention provides a kind of extracting method that " superbug " is had the good killing effect sterilization original liquid.
The technical solution used in the present invention is:
A kind of method of from read the leaf seeds, extracting sterilization original liquid, described method comprises:
(1) fetches phytoclasts from broad-leaved tree, be crushed to 30~100 orders, the dry dried powder that gets, with dried powder be added to soak 5~8 hours in the water that quality is 20~35 times of dried powder quality after, adding quality is the magnesium sulfate or the potassium sulphate of dried powder quality 0.02%~10%, and add sodium hydroxide or potassium hydroxide regulator solution pH value is 8~12, be warming up to 80~100 ℃ of insulation 60~90min, filter, filter residue adds the water of 5~10 times of filter residue quality, transfer pH to 8~12 with sodium hydroxide or potassium hydroxide, in 80~100 ℃ of insulation lixiviate 60~90min, filter, merging filtrate obtains extract just;
(2) first extract is in 68~88 ℃ of bottom fermentations, milk yellow appears in zymotic fluid or pink crystallization (needs 10~30 days usually, through repetition test repeatedly, find whether to occur in the zymotic fluid crystallization and extract whether successful important indicator for judging, if milk yellow or pink crystallization do not occur, the then final material that obtains that extracts is the energy that do not have microbe killing properties), turn 2~3 every day between yeast phase, and fermentation ends is filtered and is obtained zymotic fluid;
(3) zymotic fluid places evaporator, keeps temperature to be 85~110 ℃ and carries out steam separation 8~10 hours, and the remaining liq cooling obtains described sterilization original liquid.
Described broad-leaved tree is common broad-leaved tree seeds, can be one of following or wherein two or more mixing: cypress CupressusfunebrisEndl (Cupressaceae), teak Tectona grandis Verbenaceae (Verenaceae), Korean pine Pinus koraiensis Sieb.et Zucc (Pinaceae), white birch Betulaplatyphylla Suk. (Betulaceae), hard maple wood Acer spp.A.saccharum A.nigrumAceraceae (Aceraceae), soft maple wood Acerrubrum.A.saccharum Aceraceae (Aceraceae), Milan Aglaia spp.Mcliaccae (Meliaceae), shield seed wood Bagassa guianensisApocynaceae (Apocynaceae), LIGNUM SAPPAN Balfourdend ron rieddlianan Leguminosae (pulse family) Guntambu Betulaspp.Rutaceae (Rutaceae), light Bao Di beans Brosimumalicastrum Leguminosae (pulse family), green handle mulberry chlorophora spp.Moraceae (Moraceae), China fir Cunningha mia lanceolata Taxodiaceae (Taxodiaceae), twin columns bush Dicoryniaguianensis Leguminosae (pulse family), kapur Dipterocarp usspp Dipterocarpaceae (Dipterocarpaceae), the fragrant Dryobalano ps spp Dipterocarpa ceae (Dipterocarpaceae) of borneol, Entandrophragma cylindricum Sprague Entandr ophragma cylindricum Meliaceae (Meliaceae), red gum Eucalyptus spp Myrtaccae (Myrtaceae), Pontianak iron camphor tree Eusideroxyl on zwageriLauraceae (Lauraceae), beech Fagus spp Fagaceae (the fragrant section of shell), Manchurian ash Fraxinusmandshurica Oleaceae (Oleaceae), appoint loud, high-pitched sound to coat with lacquer wooden Glutaspp.Melanochyl a spp.melanorrhoea Anacardiaceae (Anacardiaceae), light hopea hainanensis Hopea spp Dipterocarpaceae (Dipterocarpaceae), seal eggplant Intsia spp.Leguminosae (pulse family), Ke Ku wood Kokoonaspp.Celastraceae (Wei Yuke), sweet crotons Koompassia spp.Leguminosae (pulse family), sub-capital Madhuca spp Sapotaceae (Sapotaceae), U.S. pigeonpea pericopsis sppLeguminosae (pulse family), red oak Querces spp Fagaceae (Fagaceae), the wooden Rhodoleia spp of red bud Hamamelida ceae (Hamamelidaceae), heavy red Suo Luo Shuan (being beautiful wingceltis) Shoreaspp Dipterocarpa ceae (Dipterocarpaceae), ant wood Tabebuia spp Bignoniaceae (Bignoniaceae), five-leaved chasts tree vitex quinata Verbenaceae (Verenaceae), pyinkado xyliaSpp Leguminosae (pulse family), lignum cinnamomi camphorae Cinnamonum camphora (L.) Presl (Lauraceae), rosewood 0rmosia henryi Prain (pulse family), face cream pigeonpea (being red santal) Myroxylinbalsamum Leguminosae (pulse family), Chamaecyparis formosensis Chamaecyparis formosensis (Cupressaceae).
Described phytoclasts can be preferably root and/or stem from broad-leaved tree from root, stem (comprising bark, trunk), leaf, shell, flower or the material secretion of broad-leaved tree.
Preferably, raw material deciduous species of the present invention are one of following or wherein two or more combinations: cypress CupressusfunebrisEndl, teak Tectona grandis Verbenaceae, lignum cinnamomi camphorae Cinnamonum camphora (L.) Presl, rosewood 0rmosia henryi Prain, heavy red Suo Luo Shuan Shoreaspp Dipterocarpa ceae, kapur Dipterocarp usspp Dipterocarpaceae, face cream pigeonpea Myroxylin balsamum Leguminosae, Chamaecyparis formosensis Chamaecyparisformosensis, Korean pine Pinus koraiensis Sieb.et Zucc, white birch Betula platyphyllaSuk..
Concrete, described method is as follows:
(1) fetches phytoclasts from the broad-leaved tree root, described phytoclasts is from cypress, teak, lignum cinnamomi camphorae, rosewood, heavy red Suo Luo Shuan, kapur, the phytoclasts of face cream pigeonpea root was with mass ratio 3: 2: 2: 1: 1: 0.5: 0.5 mixture, phytoclasts is crushed to 30 orders, dry dried powder, with dried powder be added to soak 5~8 hours in the water that quality is 25~30 times of dried powder quality after, adding quality is the magnesium sulfate or the potassium sulphate of dried powder quality 0.02%~10%, and add sodium hydroxide or potassium hydroxide regulator solution pH value is 8~10, be warming up to 90~100 ℃ of insulation 60~80min, filter, the filter residue water of 5~10 times of filter residue quality, transfer pH to 8~10 with sodium hydroxide or potassium hydroxide, in 90~100 ℃ of insulation lixiviate 60~80min, filter, merging filtrate obtains extract just;
(2) extract is in 68~88 ℃ of bottom fermentations, occurs in zymotic fluid that turn 2~3 every day between milk yellow or pink crystallization yeast phase, and fermentation ends is filtered and obtained zymotic fluid;
(3) zymotic fluid places evaporator, keeps temperature to be 85~110 ℃ and carries out steam separation 8~10 hours, and the remaining liq cooling promptly obtains described sterilization original liquid.
Perhaps, described method is as follows:
(1) fetches phytoclasts from the broad-leaved tree root, described phytoclasts is from cypress, teak, the phytoclasts of lignum cinnamomi camphorae root is with 1: 1: 3 mixture of mass ratio, phytoclasts is crushed to 30 orders, dry dried powder, with dried powder be added to soak 5~8 hours in the water that quality is 25~30 times of dried powder quality after, adding quality is the magnesium sulfate or the potassium sulphate of dried powder quality 0.02%~10%, and add sodium hydroxide or potassium hydroxide regulator solution pH value is 8~10, be warming up to 90~100 ℃ of insulation 60~80min, filter, filter residue adds the water of 5~10 times of filter residue matter, transfer pH to 8~10 with sodium hydroxide or potassium hydroxide, in 90~100 ℃ of insulation lixiviate 60~80min, filter, merging filtrate obtains extract just;
(2) just extract milk yellow or pink crystallization occur in 68~88 ℃ of bottom fermentations in zymotic fluid, and turn 2~3 every day between yeast phase, and fermentation ends is filtered and obtained zymotic fluid;
(3) zymotic fluid places evaporator, keeps temperature to be 85~110 ℃ and carries out steam separation 8~10 hours, and the remaining liq cooling obtains described sterilization original liquid.
Broad-leaved tree sterilization original liquid of the present invention extracts from forest plants, preparation process can not cause environmental pollution, safety non-toxic, detect proof, this extract can be eliminated " superbug ", because " superbug " has no resistance to it, so this extract is the jinx of " superbug ".This sterilization original liquid can be prepared into the natural antibacterial dye liquor and be used for textile dyeing, and the part fabric is not only nontoxic after dyeing through the natural antibacterial dye for preparing, and has antibacterial functions.And advocate under nontoxic, as to have the health care consumer goods tide impact current people, it will have vast potential for future development.
Beneficial effect of the present invention is mainly reflected in: extract the sterilization original liquid that obtains according to the inventive method " superbug " had strong killing action, at clothes, daily use chemicals, field of medicaments great role is arranged, have a extensive future.
(5) embodiment
The present invention is described further below in conjunction with specific embodiment, but protection scope of the present invention is not limited in this:
Embodiment 1: sterilization original liquid extracts
1, get cypress, teak, lignum cinnamomi camphorae, rosewood, heavy red Suo Luo Shuan, kapur, the phytoclasts of face cream pigeonpea root was with mass ratio 3: 2: 2: 1: 1: 0.5: 0.5 mixture, phytoclasts is crushed to 30 orders, dry dried powder, after soaking 8 hours in the water with dried powder 2kg adding 50kg, the magnesium sulfate that adds quality 0.02kg, and adding sodium hydrate regulator solution pH value is 9, be warming up to 90~100 ℃ of insulation 80min, filter, filter residue adds the water of 8 times of filter residue quality, transfer pH to 9 with sodium hydroxide, in 90~100 ℃ of insulation lixiviate 80min, filter, merging filtrate obtains extract just;
2, first extract is in 80 ℃ of bottom fermentations, and turn 2 every day between yeast phase, occurs pink crystallization in the time of about 30 days in the zymotic fluid, stops fermentation, filters and obtains zymotic fluid;
3, zymotic fluid places evaporator shown in Figure 1, open the preheater of evaporator, open the steam valve of evaporator top simultaneously, closing liquid outlet valve, keep temperature to be 90~100 ℃ and carry out the steam separation after 10 hours, open the liquid outlet valve of base of evaporator, begin to cool down, cooling finishes and obtains described sterilization original liquid.
Embodiment 2:
1, the phytoclasts of getting rosewood, kapur, face cream pigeonpea, Chamaecyparis formosensis stem was with mass ratio 3: 3: 2: 2 mixture, with phytoclasts be crushed to 30 orders, dry dried powder, after soaking 6 hours in the water with dried powder 2kg adding 40kg, the potassium sulphate that adds 0.1kg, and adding sodium hydrate regulator solution pH value is 10, be warming up to 90~100 ℃ of insulation 60min, filter, filter residue is with the water of filter residue 6 times of quality, transfer pH to 10 with potassium hydroxide, in 90~100 ℃ of insulation lixiviate 60min, filter, merging filtrate obtains extract just;
2, first extract is in 85 ℃ of bottom fermentations, and turn 2 every day between yeast phase, the milk yellow crystallization occurs in the zymotic fluid in the time of about 20 days, stops fermentation, filters and obtains zymotic fluid;
3, zymotic fluid places evaporator, open branch road pump, preheating and the heater of evaporator, open the valve of vapour separator simultaneously, keep temperature to be 100~110 ℃ and carry out the steam separation after 8 hours, open the liquid outlet valve of base of evaporator, begin to cool down, cooling finishes and obtains described sterilization original liquid.
Embodiment 3:
1, gets the phytoclasts of cypress, teak, lignum cinnamomi camphorae root with 1: 1: 3 mixture of mass ratio, with phytoclasts be crushed to 30 orders, dry dried powder, after soaking 8 hours in the water with dried powder 1.5kg adding 45kg, the potassium sulphate that adds 0.03kg, and adding potassium hydroxide regulator solution pH value is 8, be warming up to 90~100 ℃ of insulation 80min, filter, filter residue is with the water of 10 times of filter residue quality, transfer pH to 8 with potassium hydroxide, in 90~100 ℃ of insulation lixiviate 80min, filter, merging filtrate obtains extract just;
2, first extract is in 75 ℃ of bottom fermentations, and turn 2 every day between yeast phase, the milk yellow crystallization occurs in the time of about 30 days, stops fermentation, and fermentation ends is filtered and obtained zymotic fluid;
3, zymotic fluid places evaporator, open the preheater of evaporator, open the steam valve of evaporator top simultaneously, closing liquid outlet valve, keep temperature to be 85~98 ℃ and carry out the steam separation after 10 hours, open the liquid outlet valve of base of evaporator, begin to cool down, cooling finishes and obtains described sterilization original liquid.
Embodiment 4:
1, gets the mixture of the phytoclasts of cypress root and rosewood stem with mass ratio mixing in 4: 1, with phytoclasts be crushed to 30 orders, dry dried powder, after soaking 8 hours in the water with dried powder 2kg adding 55kg, the potassium sulphate that adds 0.08kg, and adding sodium hydrate regulator solution pH value is 9, be warming up to 90~100 ℃ of insulation 80min, filter, filter residue is with the water of filter residue quality 10, with sodium hydroxide accent pH to 9, in 90~100 ℃ of insulation lixiviate 80min, filter, merging filtrate obtains extract just;
2, first extract is in 85 ℃ of bottom fermentations, and turn 2 every day between yeast phase, the milk yellow crystallization occurs in the time of about 20 days, stops fermentation, filters and obtains zymotic fluid;
3, zymotic fluid places evaporator, open the preheater of evaporator, open the steam valve of evaporator top simultaneously, closing liquid outlet valve, keep temperature to be 90~100 ℃ and carry out the steam separation after 10 hours, open the liquid outlet valve of base of evaporator, begin to cool down, cooling finishes and obtains described sterilization original liquid.
Embodiment 6:
1, get hard maple wood, soft maple wood, Milan, shield seed wood, Guntambu, the phytoclasts of balsam wood beanstalk portion was with mass ratio 3: 3: 1: 1: 1: 1 mixture, phytoclasts is crushed to 30 orders, dry dried powder, after soaking 6 hours in the water with dried powder 2kg adding 40kg, the potassium sulphate that adds 0.15kg, and adding sodium hydrate regulator solution pH value is 10, be warming up to 90~100 ℃ of insulation 80min, filter, it is the water of 6 times of filter residue quality that filter residue adds quality, transfer pH to 10 with potassium hydroxide, in 90~100 ℃ of insulation lixiviate 80min, filter, merging filtrate obtains extract just;
2, first extract is in 85 ℃ of bottom fermentations, and turn 2 every day between yeast phase, the milk yellow crystallization occurs in the zymotic fluid in the time of about 21 days, stops fermentation, filters and obtains zymotic fluid;
3, zymotic fluid places evaporator, open the preheater of evaporator, open the steam valve of evaporator top simultaneously, closing liquid outlet valve, keep temperature to be 100~110 ℃ and carry out the steam separation after 8 hours, open the liquid outlet valve of base of evaporator, begin to cool down, cooling finishes and obtains described sterilization original liquid.
Embodiment 7:
1, get LIGNUM SAPPAN, China fir, kapur, Korean pine, white birch, red oak, the phytoclasts of ant wood root was with mass ratio 3: 2: 2: 1: 1: 0.5: 0.5 mixture, phytoclasts is crushed to 30 orders, dry dried powder, after soaking 8 hours in the water with dried powder 2kg adding 50kg, the magnesium sulfate that adds 0.05kg, and adding sodium hydrate regulator solution pH value is 9, be warming up to 90~100 ℃ of insulation 80min, filter, filter residue adds the water of 8 times of filter residue quality, transfer pH to 9 with sodium hydroxide, in 90~100 ℃ of insulation lixiviate 80min, filter, merging filtrate obtains extract just;
2, first extract is in 80 ℃ of bottom fermentations, and turn 2 every day between yeast phase, occurs pink crystallization in the time of about 32 days in the zymotic fluid, stops fermentation, filters and obtains zymotic fluid;
3, zymotic fluid places evaporator, open the preheater of evaporator, open the steam valve of evaporator top simultaneously, closing liquid outlet valve, keep temperature to be 90~100 ℃ and carry out the steam separation after 10 hours, open the liquid outlet valve of base of evaporator, begin to cool down, cooling finishes and obtains described sterilization original liquid.
Embodiment 8:
1, gets the phytoclasts of China fir, borneol perfume (or spice), red gum root with 1: 1: 3 mixture of mass ratio, with phytoclasts be crushed to 30 orders, dry dried powder, after soaking 8 hours in the water with dried powder 1.5kg adding 45kg, the potassium sulphate that adds 0.06kg, and adding potassium hydroxide regulator solution pH value is 8, be warming up to 90~100 ℃ of insulation 80min, filter, filter residue is with the water of filter residue 10 times of quality, transfer pH to 8 with potassium hydroxide, in 90~100 ℃ of insulation lixiviate 80min, filter, merging filtrate obtains extract just;
2, first extract is in 75 ℃ of bottom fermentations, and turn 2 every day between yeast phase, the milk yellow crystallization occurs in the time of about 28 days, stops fermentation, and fermentation ends is filtered and obtained zymotic fluid;
3, zymotic fluid places evaporator, open the preheater of evaporator, open the steam valve of evaporator top simultaneously, closing liquid outlet valve, keep temperature to be 85~98 ℃ and carry out the steam separation after 10 hours, open the liquid outlet valve of base of evaporator, begin to cool down, cooling finishes and obtains described sterilization original liquid.
Embodiment 9:
1, gets the mixture of the phytoclasts of green handle mulberry root and twin columns bush stem with mass ratio mixing in 4: 1, with phytoclasts be crushed to 30 orders, dry dried powder, after soaking 8 hours in the water with dried powder 2kg adding 55kg, the magnesium sulfate that adds 0.08kg, and adding sodium hydrate regulator solution pH value is 9, be warming up to 90~100 ℃ of insulation 80min, filter, filter residue add 10 times of quality of filter residue water, transfer pH to 9 with sodium hydroxide, in 90~100 ℃ of insulation lixiviate 80min, filter, merging filtrate obtains extract just;
2, first extract is in 85 ℃ of bottom fermentations, and turn 2 every day between yeast phase, the milk yellow crystallization occurs in the time of about 25 days, stops fermentation, filters and obtains zymotic fluid;
3, zymotic fluid places evaporator, open the preheater of evaporator, open the steam valve of evaporator top simultaneously, closing liquid outlet valve, keep temperature to be 90~100 ℃ and carry out the steam separation after 10 hours, open the liquid outlet valve of base of evaporator, begin to cool down, cooling finishes and obtains described sterilization original liquid.
Embodiment 10~15:
Get cypress, teak, lignum cinnamomi camphorae, rosewood, kapur, Chamaecyparis formosensis root phytoclasts respectively, be crushed to 30 orders, dry dried powder, respectively get the 2kg dried powder and extract sterilization original liquid according to embodiment 1 method, the gained sterilization original liquid carries out the bactericidal effect experiment.
Embodiment 11: the bactericidal effect experiment
(1) test item and test basis:
" disinfection technology standard " version 2.1.1.7 in 2002 bacteria quantified is killed experiment
(2) test strain:
Staphylococcus aureus: ATCC No.6538 (gram-positive bacteria)
(3) method step:
1, get embodiment 1~15 sterilization original liquid, be mixed with the 250mg/L thimerosal with sterile water respectively, it is standby to put 20 ℃ ± 1 ℃ water-bath;
2, the staphylococcus aureus compound concentration 5 * 10
3The bacteria suspension of cfu/mL;
3, the aseptic Boiling tube of cancellation poison test adds the 0.5mL bacteria suspension earlier, adds 0.5mL bovine serum albumin (0.5mg/mL) again, mixing, insert in 20 ℃ ± 1 ℃ water-bath behind the 5min, draw each 4.0mL of above-mentioned thimerosal with aseptic straw and inject wherein, mixing and timing immediately rapidly;
4, treat that experimental bacteria and thimerosal interacted to the scheduled time, draw the mixed liquor 0.5mL of experimental bacteria and thimerosal respectively, be added to 4.5mL in the inorganic agent (sulfuric acid phenol sodium and soybean lecithin mixture, sulfur acid phenol sodium 0.5g) of sterilization, mixing;
5, respectively manage treated dose of mixed liquor effect 10min after, draw 1.0mL sample liquid respectively, measure by the bacterial culture method of counting and deposit viable count, 2 plates of every pipe sample liquid inoculation.As the bacterium number of growing on the flat board more for a long time, can carry out 10 times of dilutions after, carry out viable bacteria again and cultivate counting.
6, replace thimerosal with sterile water simultaneously, carry out parallel test according to step 3~5 operations, as positive control;
7, all test samples are all cultivated in 37 ℃ of incubators, and test repeats 3~4 times, calculate the viable bacteria concentration (cfu/mL) of each pipe, and calculate sterilizing rate with reference to the viable bacteria concentration of positive control.
(4) assay
See Table 1.
Table 1
By table 1 as seen, the bacteriostasis rate of deciduous species extract all reaches more than 96%, this shows that the sterilization original liquid that extracts with broad-leaved tree has the good restraining effect to staphylococcus aureus (" superbug "), and it is nontoxic to human body, can be applicable to clothes, daily use chemicals, medicine and other fields, have broad prospect of application.