CN105001991A - Ledum palustre extractive with sterilization function and preparing method and application thereof - Google Patents
Ledum palustre extractive with sterilization function and preparing method and application thereof Download PDFInfo
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- CN105001991A CN105001991A CN201510331271.XA CN201510331271A CN105001991A CN 105001991 A CN105001991 A CN 105001991A CN 201510331271 A CN201510331271 A CN 201510331271A CN 105001991 A CN105001991 A CN 105001991A
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Abstract
The invention discloses a ledum palustre extractive with a sterilization function and a preparing method and application thereof. The preparing method comprises the steps that ledum palustre broken particles are placed in an extraction tank, then the extraction tank is heated through a water circulation system, and the extraction tank and a separation tank are vacuumized through heating by means of a vacuum circulating system; extraction agent liquefied butane is pumped into the extraction tank till the ledum palustre broken particles can be submerged by the extraction agent; when the temperature of the extraction tank reaches 25-65 DEG C and the pressure of the extraction tank reaches 0.3-0.7 Mpa, electric heating and hot oil pump circulation are stopped, and the water circulation system is stopped; after extraction is conducted for 0.5-2 hours, the extraction agent is recovered, a recovering loop is closed, a compressor and a refrigerator are started, and recovering is completed when it is observed that no liquid flows downwards from a window; extracted ledum palustre extractive extractum is obtained from the separation tank. The ledum palustre extractive with the sterilization function and the preparing method and application thereof have the advantages that equipment is simple, operation is easy, the extraction rate is high, the extractive is nontoxic and harmless, the recovery rate of solvent is high, and the selectivity is good.
Description
Technical field
The present invention relates to plant milk extract field, specifically, is a kind of Du Xiang extract with germicidal action and preparation method thereof.
Background technology
Du Xiang (Ledum palustre L.) is the wild plant resource that China's Daxinganling District accumulation is abundant, and research data both domestic and external all shows that it has important spices and is worth and pharmaceutical use, urgently develops.Du Xiang branches and leaves, flowers and fruits are all containing volatile aromatic oil, and its main component is for Du is aromatic, come into leaves pine camphor, cymene etc.Ledum palustre L. var. dilatatum Wahl.oil has antibechic, eliminates the phlegm, and relievings asthma, pharmacological effect that step-down, vasodilation, sterilizing and itch-relieving, short skin absorb.In Du Xiang volatile oil capsule, cymene content is greater than 80%, is used for the treatment of chronic tracheitis.The northern China Mongols and Korean nationality using Du Xiang as traditional national medicine simply, another name Leaf of Narrowleaf Cryslatlea Ledum, loudspeaker tea.Branch, leaf are used as medicine, and conventional use is: " Leaf of Narrowleaf Cryslatlea Ledum leaf is appropriate, and decocting filters, and is condensed into cream, takes the circumstances into consideration for oral administration ", cures mainly " promoting blood flow to regulate menstruation; Preventing phlegm from forming and stopping coughing "; Or " Leaf of Narrowleaf Cryslatlea Ledum 3 money decocting, day takes secondary, controls stomach ulcer ".Visible, its conventional use is hot water extraction, concentrated processing.Modern biology research also proves that Du Xiang aqueous extract has anti-oxidant, to prevent radiation injury effect.30min after Du's volatile oil volatilizees in atmosphere naturally, have the effect significantly killing bacterium in air, after different volatilizes, kill the effect of bacterium in air without significant difference, sterilizing ability is relevant with the concentration of volatile oil of shutting out in air.Research finds that the growth of Du Xiang volatile oil to insect black peach aphid, cotten aphid of methanol extraction is inhibited, give tested material 24,28, after 72h, the survival rate of black peach aphid and cotten aphid is respectively 45.0%, 31.9%, 23.6% and 3.7%, 13.1%, 10.9%.Have the very special smell of one after the burning of Du Xiang branches and leaves, China's normal way of burning Du Xiang fumigating chamber house that utilizes among the people carrys out the insects such as extinguishing bugs, moth, cockroach.Current production is extracted the method mainly vapor distill extraction method of essential oil from Du Xiangzhong.The extraction time of this method is longer, and essential oil yield is low.
Vibrio parahaemolyticus (Vibrio parahaemolyticus) is a kind of halophilic bacterium be widely distributed in bay all over the world and region, shoreline and sea-food.This bacterium is a kind of conditioned pathogen, under certain condition can outbreak of epidemic.In recent years, along with going from bad to worse of breeding environment, the report that China's Coastal Areas causes sea-food morbidity or Large Scale Death and human foods poisoning because of Vibrio parahemolyticus is increasing.Current known Vibrio parahaemolyticus can cause Chinese prawn red leg disease, large yellow croaker, cabrilla septicemia, oyster, Haliotis diversicolor muscular dystrophy and can also infect cultivated crabs class, causes the mortality of cultivated crabs class; Infect the mankind by contaminated sea-food simultaneously, cause human intestine's acute infectious disease.Therefore, can say that Vibrio parahaemolyticus is ocean aquatic economic animal vibriosis the main pathogenic fungi, be also the enemy of human food prods's safety.Vibrio parahaemolyticus disease has breaks out fast, popular wide, mortality ratio high, because bacterium very easily develops immunity to drugs to microbiotic, therefore current to Vibrio parahaemolyticus disease also not specific methods for the treatment of.
Vibrio alginolyticus (Vibrio alginolyticus) belongs to vibrionaceae (Vibrionaceae), Vibrio (Vibrio), Gram-negative tyrothricin, be distributed widely in seawater and river mouth place all over the world, and quantity occupies first of seawater class vibrios.Vibrio alginolyticus is present in multiple marine animal, is the conditioned pathogen of the marine cultured animal such as fish, shrimp.Vibrio alginolyticus, it mostly occurs in summer to the pathogenic of cultivated animals, easily popular at water temperature 25 ~ 32 DEG C, also easily occurs in addition when the decline of animal body immunity function or environmental degradation.In addition vibrio alginolyticus also has a large amount of reports to the pathogenic of people, can cause that people poisons by food, otitis etc.
Summary of the invention
The technical problem solved: the invention provides a kind of Du Xiang extract with germicidal action and its preparation method and application.
Technical scheme: a kind of preparation method with the Du Xiang extract of germicidal action, preparation process is as follows: in extractor, load 20 ~ 60 object Du Xiang particles, then by water circulation system, extractor is heated, through heating, when making the temperature of extractor reach 25 DEG C ~ 65 DEG C, vacuum cycle system is utilized to vacuumize extractor and separating tank, when its vacuum tightness reaches-0.08Mpa ~-0.06Mpa, valve-off, closes vacuum pump; Extraction agent liquefied butane is pumped into, until extraction agent can flood Du Xiang particle in extractor; When the temperature of extractor reach 25 DEG C ~ 65 DEG C, pressure reach 0.3Mpa ~ 0.7Mpa time, stop electrically heated and hot oil pump to circulate, closedown water circulation system; After extraction 0.5 ~ 2h, reclaim extraction agent, open recovery passage, open compressor and refrigerator, when observation window absence of liquid flows down, reclaim complete; From the Du Xiang extract medicinal extract that separating tank is extracted.
The above-mentioned preparation-obtained Du Xiang extract with germicidal action.
Above-mentioned Du Xiang extract suppresses the Vibrio parahaemolyticus in seawater and/or the application in vibrio alginolyticus medicine in preparation.
Vibrio parahaemolyticus in suppression seawater and/or the medicine of vibrio alginolyticus, effective constituent is the above-mentioned Du Xiang extract prepared.
Beneficial effect: the Du Xiang medicinal extract quality that the present invention extracts is good, and extraction yield is high, can extract 4.0%, and extraction time is short, and extraction agent recycle efficiency is high, environmentally safe, is a kind of Chemical Engineering Technology of environmental protection.The Du Xiang extract that the present invention prepares has extremely strong restraining effect to the Vibrio parahaemolyticus in seawater and vibrio alginolyticus.
Accompanying drawing explanation
Fig. 1: subcritical abstraction tripping device of the present invention and process flow sheet;
The SPE-GC-MS of Fig. 2: Du Xiang medicinal extract analyzes collection of illustrative plates;
Fig. 3: embodiment 1 gained Du Xiang extract is to sterilization effect (the A1 seawater stoste dilution 10 of bacterium in seawater
-1doubly, A2 seawater stoste dilution 10
-2doubly, A3 seawater stoste dilution 10
-3doubly, B1, B2, B3 add concentration 5g/L Du Xiang extract, and C1, C2, C3 add concentration 10g/L Du Xiang extract, and D1, D2, D3 add concentration 15g/L Du Xiang extract).
Embodiment
With embodiment, the invention will be further described below, but the present invention is not limited to these embodiments.
Embodiment 1:
In extractor, load 2.314kg granularity is 60 object Du Xiang branches and leaves particles, then by water circulation system, extractor is heated, through heating, when the actual temperature of experiment reaches 50 DEG C, vacuum cycle system is utilized to vacuumize extractor and separating tank, when its vacuum tightness reaches-0.08Mpa, valve-off, closes vacuum pump.Secondly in extractor, extraction agent liquefied butane is pumped into, until extraction agent can flood Du's perfume material.Again, see thermometer and the tensimeter of extractor, when temperature reach temperature required 50 DEG C ~ 60 DEG C of experiment, pressure reach 0.5Mpa ~ 0.7Mpa time, stop electrically heated and hot oil pump to circulate, closedown water circulation system.Timing, after extraction 1h, reclaims extraction agent, opens recovery passage, start compressor and refrigerator, when observation window absence of liquid flows down, reclaim complete.The last Du Xiang medicinal extract be extracted from separating tank.Through weighing as 90g, be yellow medicinal extract.Its extraction yield is 4.0%.Measure (see Fig. 2) through SPE-GC-MS, the volatile component of its Du Xiang medicinal extract has 56 kinds (see table 1).
Embodiment 2:
In extractor, load 2.443kg granularity is 20 object Du Xiang branches and leaves particles, then by water circulation system, extractor is heated, through heating, when the actual temperature of experiment reaches 40 DEG C, vacuum cycle system is utilized to vacuumize extractor and separating tank, when its vacuum tightness reaches-0.08Mpa, valve-off, closes vacuum pump.Secondly in extractor, extraction agent liquefied butane is pumped into, until extraction agent can flood Du's perfume material.Again, see thermometer and the tensimeter of extractor, when temperature reach temperature required 40 DEG C ~ 50 DEG C of experiment, pressure reach 0.3Mpa ~ 0.7Mpa time, stop electrically heated and hot oil pump to circulate, closedown water circulation system.Timing, after extraction 1h, reclaims extraction agent, opens recovery passage, start compressor and refrigerator, when observation window absence of liquid flows down, reclaim complete.The last Du Xiang medicinal extract be extracted from separating tank.Through weighing as 120g, be yellow medicinal extract.Its extraction yield is 4.91%.Measure through SPE-GC-MS, the volatile component of its Du Xiang medicinal extract has 56 kinds.
Embodiment 3:
In extractor, load 2.37kg granularity is 20 object Du Xiang branches and leaves particles, then by water circulation system, extractor is heated, through heating, when the actual temperature of experiment reaches 40 DEG C, vacuum cycle system is utilized to vacuumize extractor and separating tank, when its vacuum tightness reaches-0.08Mpa, valve-off, closes vacuum pump.Secondly in extractor, extraction agent liquefied butane is pumped into, until extraction agent can flood Du's perfume material.Again, see thermometer and the tensimeter of extractor, when temperature reach temperature required 40 DEG C ~ 50 DEG C of experiment, pressure reach 0.3Mpa ~ 0.7Mpa time, stop electrically heated and hot oil pump to circulate, closedown water circulation system.Timing, after extraction 1h, reclaims extraction agent, opens recovery passage, start compressor and refrigerator, when observation window absence of liquid flows down, reclaim complete.The last Du Xiang medicinal extract be extracted from separating tank.Through weighing as 126g, be yellow medicinal extract.Its extraction yield is 5.31%.Measure through SPE-GC-MS, the volatile component of its Du Xiang medicinal extract has 56 kinds.
Main chemical compositions in table 1 Du Xiang medicinal extract
Embodiment 4: Du Xiang extract is tested the germicidal action of aquaculture water
1. experimental technique
The cultivation of 1.1 pathogenic bacterium
Cultivate under Vibrio parahaemolyticus (Vibrio parahaemolyticus) and Vibrio alginnolyficus (Vibrio alginolyticus) 37 DEG C of conditions.Tryptose soya agar (TSA) Tryptic Soy Agar fills a prescription: (g/L) Tryptones 15.0g, soy peptone 5.0g, sodium-chlor 5.0g, agar 15.0g, pH value 7.3.After taking, heated and stirred is dissolved in distilled water, packing triangular flask, and 121 DEG C of autoclavings, are down flat plate.Pancreas peptone soybean broth substratum (TSB) Tryptic soy Broth, does not add agar, and other is according to tryptose soya agar (TSA) Tryptic Soy Agar recipe configuration.Incubated overnight under 37 DEG C of conditions.
Vibrio alginolyticus culture condition is the same with Vibrio parahaemolyticus.
The inoculation of 1.2 bacteriums
The pathogenic bacterium of 100 μ L are inoculated into respectively and with the addition of three different concns (5g/L, 10g/L, 15g/L) and extract in the seawater of the Du Xiang extract obtained through embodiment 1, then the seawater of each concentration is done 10 respectively
-1, 10
-2, 10
-3the dilution of three gradients, shakes up, and the bacterium liquid then getting 10 μ L is respectively inoculated on tryptose soya agar (TSA) substratum, under 37 DEG C of conditions, then carry out the cultivation 24h of bacterium.
The counting of 1.3 bacterium colonies
Cultured flat-plate bacterial colony bacterial count instrument is counted.
2. experimental result
| Dilution 10 ‐1Doubly | Dilution 10 ‐2Doubly | Dilution 10 ‐3Doubly |
| Seawater stoste | ** | ** | 500 |
| Add 5g/L concentration | ** | 12 | 5 |
| Add 10g/L concentration | ** | 15 | 12 |
| Add 15g/L concentration | ** | 20 | 8 |
Note: * * represents that colony number is more than 2000
As can be seen from experimental result, three dilution gradients of seawater stoste normally can turn out pathogenic bacterium when not adding extract, the bacterium liquid energy normal growth in seawater is described.And three concentration samples adding Du Xiang extract all create extremely strong restraining effect to the Vibrio parahaemolyticus in seawater and vibrio alginolyticus.And Du Xiang extract add concentration be 5g/L time to the inhibition of pathogenic bacterium best (see Fig. 3).
The invention is not restricted to above-described embodiment, all can implement described in content of the present invention and there is described good result.
Claims (4)
1. there is a preparation method for the Du Xiang extract of germicidal action, it is characterized in that preparation process is as follows:
(1) in extractor, 20 ~ 60 object Du Xiang particles are loaded, then by water circulation system, extractor is heated, through heating, when making the temperature of extractor reach 25 DEG C ~ 65 DEG C, vacuum cycle system is utilized to vacuumize extractor and separating tank, when its vacuum tightness reaches-0.08 Mpa ~-0.06 Mpa, valve-off, closes vacuum pump;
(2) in extractor, extraction agent liquefied butane is pumped into, until extraction agent can flood Du Xiang particle;
(3) when the temperature of extractor reach 25 DEG C ~ 65 DEG C, pressure reach 0.3 Mpa ~ 0.7 Mpa time, stop electrically heated and hot oil pump to circulate, closedown water circulation system;
(4) after extracting 0. 5 ~ 2 h, reclaim extraction agent, open recovery passage, open compressor and refrigerator, when observation window absence of liquid flows down, reclaim complete;
(5) from the Du Xiang extract medicinal extract that separating tank is extracted.
2. the preparation-obtained Du Xiang extract with germicidal action of claim 1.
3. Du Xiang extract according to claim 2 suppresses the Vibrio parahaemolyticus in seawater and/or the application in vibrio alginolyticus medicine in preparation.
4. the Vibrio parahaemolyticus in suppression seawater and/or the medicine of vibrio alginolyticus, is characterized in that effective constituent is the Du Xiang extract that claim 1 prepares.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109897730A (en) * | 2019-03-18 | 2019-06-18 | 黑龙江中医药大学 | A kind of Du Xiang refined volatile oil refinement method |
| CN113136267A (en) * | 2021-05-03 | 2021-07-20 | 芭而蒂洗涤科技(天津)有限公司 | A cleaning product containing Ledum Palustre L extract and its preparation method |
| JP7366308B1 (en) * | 2023-06-09 | 2023-10-20 | 小川香料株式会社 | fragrance composition |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109897730A (en) * | 2019-03-18 | 2019-06-18 | 黑龙江中医药大学 | A kind of Du Xiang refined volatile oil refinement method |
| CN113136267A (en) * | 2021-05-03 | 2021-07-20 | 芭而蒂洗涤科技(天津)有限公司 | A cleaning product containing Ledum Palustre L extract and its preparation method |
| JP7366308B1 (en) * | 2023-06-09 | 2023-10-20 | 小川香料株式会社 | fragrance composition |
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Application publication date: 20151028 |