CN102218026B - Use of willow leaf wintersweet extract in preparation of mosquito repelling agent - Google Patents

Use of willow leaf wintersweet extract in preparation of mosquito repelling agent Download PDF

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CN102218026B
CN102218026B CN2011101589414A CN201110158941A CN102218026B CN 102218026 B CN102218026 B CN 102218026B CN 2011101589414 A CN2011101589414 A CN 2011101589414A CN 201110158941 A CN201110158941 A CN 201110158941A CN 102218026 B CN102218026 B CN 102218026B
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chimonanthus salicifolius
preparation
quintessence oil
anophelifuge
salicifolius
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CN102218026A (en
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田薇
方程吉
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Zhejiang A&F University ZAFU
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Zhejiang A&F University ZAFU
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Abstract

The invention relates to an application of a willow leaf wintersweet extract in the preparation of a mosquito repelling agent. Preferentially, the mosquito repelling agent is prepared by the following steps: taking willow leaf wintersweet leaf blades, pulverizing through a pulverizer, screening, extracting and separating for obtaining willow leaf wintersweet essential oil. The mosquito repelling agent integrates three effects, namely repelling mosquitoes, keeping moisture and protecting health, into a whole, thereby having very wide application prospect.

Description

The Chimonanthus salicifolius extract is used to prepare anophelifuge
Technical field
The present invention relates to the application that the Chimonanthus salicifolius extract prepares anophelifuge.
Background technology
Folium Salicis Babylonicae wax prunus mume (sieb.) sieb.et zucc. is half evergreen shrubs, and leaf papery or thin keratin, ovum shape lanceolar are to the ellipticity lanceolar, and tip is point gradually, the base portion wedge shape; Leaf table yellow green, following flour is green, the rough hair of petiole and blade tool: brightly yellowish white, be born in axil, etaerio of achenes and is born in the gyalectiform hypocarp, and in 12~January of florescence, fruit 5~July of next year phase is on the normal Su Cunzhi.
It is reported that the effect of Folium Salicis Babylonicae wax prunus mume (sieb.) sieb.et zucc. has: expelling summer-heat promotes the production of body fluid, and powder for improving appetite is strongly fragrant, and lactogenesis is moisturized, cough-relieving.Cure mainly the summer-heat dizziness, vomiting, stagnation of QI stomach is vexed, measles, pertussis is scalded burn, otitis media etc.Dispel the wind and regulate the flow of vital energy, promoting blood circulation and detoxication.Cure mainly asthma, the epersalgia cough, stomachache, stomachache, the pruritus due to wind-damp pathogen pain is treated pyogenic infections from tumour or sore, traumatic injuries etc.Suitable amount used externally is ground into powder and is spread etc.
At present, people's anophelifuge articles for use the most commonly used are mosquito incenses in summer, do not know that but this can damage human body.In fact, the active ingredient of most of mosquito incenses is pyrethrin insecticides, and organic filler, adhesive, dyestuff and other additives etc., therefore contains many harmful materials in the cigarette of mosquito incense burning, might bring out diseases such as asthma.According to measuring and calculating, the microgranule that point one volume mosquito incense is emitted is roughly the same with the amount of burning 100 left and right sides medicated cigarettes, and the ultrafine dust that discharges can enter and be deposited in the lung, possibly cause asthma in a short time, for a long time then maybe cause cancer.Next is the carcinogen that mosquito incense base material imperfect combustion produces, and some can stimulate the chemical compound of upper respiratory tract, and these materials can make people's nervous system poison.
Domestic application for the Chimonanthus salicifolius volatile oil component at present mainly concentrates on medicinal aspect, and do not see can driving away mosquito to it any report.He Jianyun etc. have delivered " volatile oil component analysis in the Chi monanthus salicifolius " in " chemistry with life engineering " the 27th the 4th phase of volume, wherein the component of Chimonanthus salicifolius are studied, and anyly do not report about anophelifuge but have.
Summary of the invention
Technical problem to be solved by this invention provides and a kind of the Chimonanthus salicifolius leaf extract is applied to prepare anophelifuge, and the gained anophelifuge has good repelling effect.
Technical scheme of the present invention is:
The Chimonanthus salicifolius extract is used to prepare anophelifuge.
Preferably, said anophelifuge is by the preparation of following step and get: get the Chimonanthus salicifolius blade and pulverize with pulverizer, sieve, extraction separates and must the Chimonanthus salicifolius quintessence oil.
Preferably, supercritical extraction equipment is adopted in described extraction, and supercritical extraction equipment is made up of extraction kettle and two separating stills, and extracting pressure is 21.1MPa, and extraction temperature is 54.5 ℃, and the extraction time is 1.3h; Separating still I pressure is made as 6.0MPa, temperature is made as 40 ℃; Separating still II pressure is made as 6.0MPa, and temperature is made as 40 ℃; CO 2Flow is 20L/h.
Supercritical extraction equipment of the present invention can be bought through market and get, like the HA221-50-06 type supercritical fluid extraction equipment of Huaan, Nantong supercritical extraction company production.
Preferably, said anophelifuge is got by following step preparation:
1) preparation Chimonanthus salicifolius quintessence oil: get the Chimonanthus salicifolius blade, pulverize, sieve with pulverizer, extraction, separate and the Chimonanthus salicifolius quintessence oil;
2) preparation Chimonanthus salicifolius quintessence oil clathrate: adopt saturated water solution method that the Chimonanthus salicifolius quintessence oil is processed Benexate Hydrochloride;
3) with the Pseudobulbus Bletillae polysaccharose aqueous solution of the quintessence oil clathrate that makes and 1wt%~50wt%,, fully stir into suspension and promptly get according to 1: 90~90: 1 mixed of weight ratio.
Preferably, step 2) in, the saturated aqueous solution of preparation beta-schardinger dextrin-; Selecting Chimonanthus salicifolius quintessence oil and beta-schardinger dextrin-ratio is 1: 5~10mL/g, and the enclose temperature is 40~50 ℃, and mixing time is 1~3h; Make the clathrate of Chimonanthus salicifolius quintessence oil, it is poured under stirring condition in the 10wt% aqueous solution of beta-schardinger dextrin-, stir; Sucking filtration, 40 ℃ of dry Chimonanthus salicifolius quintessence oil clathrates that get of filtering residue.
Preferably, selecting Chimonanthus salicifolius quintessence oil and beta-schardinger dextrin-usage ratio is 1: 8mL/g, and the enclose temperature is 45 ℃, mixing time is 2h, makes the clathrate of Chimonanthus salicifolius quintessence oil.
Preferably, in the step 1), the Chimonanthus salicifolius leaf is pulverized the back and is crossed 50 mesh sieves.
Preferably, supercritical extraction equipment is adopted in the extraction of step 1), and described supercritical extraction equipment is made up of extraction kettle and two separating stills, and extracting pressure is 21.1MPa, and extraction temperature is 54.5 ℃, and the extraction time is 1.31h; Separating still I pressure is made as 6.0MPa, temperature is made as 40 ℃; Separating still II pressure is made as 6.0MPa, and temperature is made as 40 ℃; CO 2Flow is 20L/h.
The anophelifuge mechanism of Chimonanthus salicifolius quintessence oil anophelifuge of the present invention is different with traditional mosquito repellent product; The tradition mosquito repellent product produces irritative gas and/or certain toxicity to the mosquito smoked kill when using; The present invention reaches the anophelifuge purpose through producing a kind of abnormal smells from the patient that mosquito is had an avoidance effect; But this abnormal smells from the patient also plays certain function of health care to human body simultaneously as far as the human body pleasant.
Chimonanthus salicifolius quintessence oil of the present invention and liquid preparation thereof directly are applied in and are used for anophelifuge on the human body skin, and recipe ingredient all derives from side effect such as natural product, nonirritant, environmental protection safety; Simultaneously, also because the mosquito-driving liquid that the Pseudobulbus Bletillae polysaccharose in the prescription makes also has certain moisture-keeping function to people's skin; Secondly, these volatile ingredients have special health-care efficacy, can absorb through the respiratory mucosa of human body, bring into play its champignon effect.
Anophelifuge of the present invention has anophelifuge, the effect of the triple effect of preserving moisture, keep healthy unification, thereby has extremely application prospects.
The specific embodiment
Below in conjunction with embodiment the present invention is done to be described in further detail, but protection scope of the present invention is not limited to this.
Embodiment 1
1) gets Chimonanthus salicifolius blade 2000g, pulverize, cross 50 mesh sieves.Place supercritical extraction equipment respectively, extraction, blood pressure lowering separate altogether 20mL Chimonanthus salicifolius quintessence oil; Described supercritical extraction equipment adopts two separating stills, and extracting pressure is 21.1MPa, and extraction temperature is 54.5 ℃, and the extraction time is 1.31h; Separating still I pressure is made as 6.0MPa, temperature is made as 40 ℃; Separating still II pressure is made as 6.0MPa, and temperature is made as 40 ℃; CO 2Flow is 20L/h.
2) adopt saturated water solution method, the ratio of Chimonanthus salicifolius quintessence oil and β-CD (beta-schardinger dextrin-) is 1: 8mL/g, and the enclose temperature is 45 ℃; Mixing time is 2h, and the ratio of β-CD and water is 1: 10g/mL makes the clathrate of Chimonanthus salicifolius quintessence oil; It is poured in the aqueous solution (wt10%) of beta-schardinger dextrin-into stir about 2 hours, cold preservation 24 hours under stirring condition; Sucking filtration, 40 ℃ of dry Chimonanthus salicifolius oil clathrates that get of filtering residue;
3) get commercially available Pseudobulbus Bletillae polysaccharose and Chimonanthus salicifolius quintessence oil clathrate, click the suspension that weight ratio is mixed with Chimonanthus salicifolius:
The Benexate Hydrochloride 20g of Chimonanthus salicifolius quintessence oil;
Pseudobulbus Bletillae polysaccharose 5g;
Distilled water is to 100mL;
Above-mentioned Pseudobulbus Bletillae polysaccharose 5g is added in the distilled water of 80mL, treat heating after the Pseudobulbus Bletillae polysaccharose swelling, stir, treat Pseudobulbus Bletillae polysaccharose dissolving postcooling, add the Benexate Hydrochloride of Chimonanthus salicifolius quintessence oil, add water to scale and fully stir into uniform suspension and promptly get.
Embodiment 2
1) gets Chimonanthus salicifolius blade 2000g, adopt steam distillation to obtain Chimonanthus salicifolius quintessence oil 10mL, add ethanol 90ml, process oil-containing solutions;
2) take by weighing beta-schardinger dextrin-(through 50 ℃ of dry 1.5h) and put into conical flask in right amount, add an amount of distilled water then, heating for dissolving is processed full Heshui solution.After the cooling, place on the magnetic stirring apparatus, slowly add oil-containing solutions at a certain temperature, stir the enclose certain hour, leave standstill, cold preservation 24h filters.With the washing with alcohol of 100mL 95%, filter, hang, 40 ℃ of dry 2h promptly get clathrate in vacuum drying oven;
3) get commercially available Pseudobulbus Bletillae polysaccharose and Chimonanthus salicifolius quintessence oil clathrate, click the suspension that weight ratio is mixed with Chimonanthus salicifolius:
The Benexate Hydrochloride 50g of Chimonanthus salicifolius quintessence oil;
Pseudobulbus Bletillae polysaccharose 10g;
Distilled water is to 100mL;
Above-mentioned Pseudobulbus Bletillae polysaccharose 10g is added in the distilled water of 80mL, treat heating after the Pseudobulbus Bletillae polysaccharose swelling, stir, treat Pseudobulbus Bletillae polysaccharose dissolving postcooling, add the Benexate Hydrochloride of Chimonanthus salicifolius quintessence oil, add water to scale and fully stir into uniform suspension and promptly get.
The repelling effect test of effect example 1 Chimonanthus salicifolius extract
Supply the examination quintessence oil, the Chimonanthus salicifolius quintessence oil that is made by embodiment 1 step 1) is mixed with the acetone soln of 15% (V/V); With the positive contrast of 95% diethyltoluamide crude oil (commercially available), with ethanol as blank.
With reference to the State Standard of the People's Republic of China, the indoor harmacological effect of agriculture chemical registration hygienic insecticide is estimated the method for repellant (GB/T17355.10-1998) and is carried out the anophelifuge experiment.
Attack test: growing * wide * high for putting into the female mosquito of Aedes albopictus that 300 4~5 ages in days are not sucked blood in the mosquito cage of 30cm * 30cm * 60cm.After wiping out mouse web portion and becoming mildewed, depilatory is applied to abdominal part, paper towel is wiped behind the 5min, rinses well with tap water, dries with cotton balls.The depilation time should be not long, otherwise can destroy the skin of mice.Test mice is fixed in the plastic plate that folds up mouse, and abdominal part is aimed at the border circular areas (diameter 2.5cm) that is put in hollow out, and extremity and tail cover skin with the tight winding of adhesive tape.To try Mus and put into mosquito cage 2min, the examination worm that comes to stop falling is qualified for attack more than 20 persons, and this Mus and this cage mosquito can be used for repellency test.
Anophelifuge test: get 12 mices and divide 4 groups, handle with above-mentioned method depilation.On the skin of abdomen that mice exposes from border circular areas (diameter 2.5cm) (losing hair or feathers); Evenly smear respectively and supply examination quintessence oil (0.1mL), the embodiment of the invention 2 manufactured goods (0.1mL), diethyltoluamide crude oil 20 μ L and dehydrated alcohol 20 μ L, will try Mus and put into mosquito cage (300 female mosquitos in the left and right sides are arranged) respectively, observe 2min; The mosquito quantity that the record thorn is stung mice; Whether every interval 1h puts into the observation of mosquito cage has mosquito bite, observes 5h altogether, observes 2min at every turn.The mice of smearing 20 μ L dehydrated alcohol with abdominal part makes the blank group, observes the attacking ability of mosquito.Calculate the Effective Vate of Protection of each group, computing formula is following:
Effective Vate of Protection (%)=(contrast mosquito thorn sting and count-be coated with test sample after mosquito thorn sting number)/blank group mosquito is stung and stings number.Experimental result such as table 1:
Table 1 test sample group, matched group and blank control group are at the Effective Vate of Protection of different time
Figure BDA0000068116380000041
Annotate: 1 group of test sample: be Chimonanthus salicifolius quintessence oil group; 2 groups of test samples: manufactured goods of the present invention; Positive controls: repellent amine crude oil; Blank control group: dehydrated alcohol.
Those data show that Chimonanthus salicifolius quintessence oil of the present invention and repellent amine are to the effect no significant difference of the female mosquito repellent of Aedes albopictus, and repelling effect is equal to mosquito repellent product traditional on the market.

Claims (10)

1. the application of Chimonanthus salicifolius leaf extract in the preparation anophelifuge is characterized in that said Chimonanthus salicifolius leaf extract is the Chimonanthus salicifolius quintessence oil.
2. the application of Chimonanthus salicifolius leaf extract according to claim 1 in the preparation anophelifuge is characterized in that, said Chimonanthus salicifolius quintessence oil is got by following step preparation: get the Chimonanthus salicifolius blade and pulverize with pulverizer, sieve, CO 2Supercritical extraction, separate and the Chimonanthus salicifolius quintessence oil.
3. the application of Chimonanthus salicifolius leaf extract according to claim 2 in the preparation anophelifuge; It is characterized in that; Supercritical extraction equipment is adopted in described extraction, and supercritical extraction equipment is made up of extraction kettle and two separating stills, and extracting pressure is 21.1MPa; Extraction temperature is 54.5 ℃, and the extraction time is 1.3h; Separating still I pressure is made as 6.0MPa, temperature is made as 40 ℃; Separating still II pressure is made as 6.0MPa, and temperature is made as 40 ℃; CO 2Flow is 20L/h.
4. the application of Chimonanthus salicifolius leaf extract according to claim 1 in the preparation anophelifuge is characterized in that said anophelifuge is got by following step preparation:
1) preparation Chimonanthus salicifolius quintessence oil: get the Chimonanthus salicifolius blade, pulverize, sieve CO with pulverizer 2Supercritical extraction, separate and the Chimonanthus salicifolius quintessence oil;
2) preparation Chimonanthus salicifolius quintessence oil clathrate: adopt saturated water solution method that the Chimonanthus salicifolius quintessence oil is processed Benexate Hydrochloride;
3) with the Pseudobulbus Bletillae polysaccharose aqueous solution of the quintessence oil clathrate that makes and 1wt%~50wt%,, fully stir into suspension and promptly get according to the mixed of weight ratio 1:90~90:1.
5. the application of Chimonanthus salicifolius leaf extract according to claim 4 in the preparation anophelifuge is characterized in that: step 2) in, the saturated aqueous solution of preparation beta-schardinger dextrin-; Selecting Chimonanthus salicifolius quintessence oil and beta-schardinger dextrin-usage ratio is 1:5~10mL/g; The enclose temperature is 40~50 ℃, and mixing time is 1~3h, makes the clathrate of Chimonanthus salicifolius quintessence oil; It is poured under stirring condition in the 10wt% aqueous solution of beta-schardinger dextrin-; Stir sucking filtration, 40 ℃ of dry Chimonanthus salicifolius quintessence oil clathrates that get of filtering residue.
6. the application of Chimonanthus salicifolius leaf extract according to claim 5 in the preparation anophelifuge; It is characterized in that: selecting Chimonanthus salicifolius quintessence oil and beta-schardinger dextrin-usage ratio is 1:8 mL/g; The enclose temperature is 45 ℃; Mixing time is 2h, makes the clathrate of Chimonanthus salicifolius quintessence oil.
7. the application of Chimonanthus salicifolius leaf extract according to claim 4 in the preparation anophelifuge is characterized in that: in the step 1), the Chimonanthus salicifolius leaf is pulverized the back and is crossed 50 mesh sieves.
8. the application of Chimonanthus salicifolius leaf extract according to claim 4 in the preparation anophelifuge; It is characterized in that: supercritical extraction equipment is adopted in the extraction of step 1); Described supercritical extraction equipment is made up of extraction kettle and two separating stills; Extracting pressure is 21.1MPa, and extraction temperature is 54.5 ℃, and the extraction time is 1.31h; Separating still I pressure is made as 6.0MPa, temperature is made as 40 ℃; Separating still II pressure is made as 6.0MPa, and temperature is made as 40 ℃; CO 2Flow is 20L/h.
9. the application of Chimonanthus salicifolius leaf extract according to claim 4 in the preparation anophelifuge; It is characterized in that: in the step (3), Pseudobulbus Bletillae polysaccharose 5g is added in the distilled water of 80mL, treat to heat, stir after the Pseudobulbus Bletillae polysaccharose swelling; Treat Pseudobulbus Bletillae polysaccharose dissolving postcooling; Add the Benexate Hydrochloride 20g of Chimonanthus salicifolius quintessence oil, add water to 100ml, fully stir into uniform suspension and promptly get.
10. the application of Chimonanthus salicifolius leaf extract according to claim 4 in the preparation anophelifuge; It is characterized in that: in the step (3), Pseudobulbus Bletillae polysaccharose 10g is added in the distilled water of 80mL, treat to heat, stir after the Pseudobulbus Bletillae polysaccharose swelling; Treat Pseudobulbus Bletillae polysaccharose dissolving postcooling; Add the Benexate Hydrochloride 50g of Chimonanthus salicifolius quintessence oil, add water to 100ml, fully stir into uniform suspension and promptly get.
CN2011101589414A 2011-06-14 2011-06-14 Use of willow leaf wintersweet extract in preparation of mosquito repelling agent Expired - Fee Related CN102218026B (en)

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CN102696704B (en) * 2012-06-12 2014-12-31 刘倚乐 Pure natural mosquito repellent
CN103284896B (en) * 2013-01-16 2015-03-04 浙江农林大学 Chimonanthus salicifolius sterilization hand washing solution and its preparation method
CN103191160A (en) * 2013-04-15 2013-07-10 丽水学院 Preparation method of chimonanthus salicifolius formula granule
CN110651798B (en) * 2018-06-29 2021-04-13 东华理工大学 Pure natural mosquito-repellent solid aromatherapy and preparation method thereof
CN111040451A (en) * 2019-12-18 2020-04-21 佛山科学技术学院 Mosquito-repelling and insect-preventing plastic product additive

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CN102068400A (en) * 2011-01-06 2011-05-25 丽水同舟药食资源科技开发有限公司 Chimonanthus salicifolius perfume and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102068400A (en) * 2011-01-06 2011-05-25 丽水同舟药食资源科技开发有限公司 Chimonanthus salicifolius perfume and preparation method thereof

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