CN103622867B - Method for preparing mosquito-repellent perfume containing natural plant essential oil - Google Patents
Method for preparing mosquito-repellent perfume containing natural plant essential oil Download PDFInfo
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- Fats And Perfumes (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention provides a mosquito-repellent perfume, in particular relates to a perfume using natural plant essential oil as a main active component, and belongs to the technical field of daily chemicals. The natural raw materials used in the perfume comprise common nepenthes, daphne odera, geranium, mint, folium eucalypti, papaya, valerian root, folium artemisiae argyi, lindera thomsonii, jasminum lanceolarium roxb, trefoil, elecampane, german camomile and cotinus coggygria. The mosquito-repellent perfume provided by the invention is prepared from natural plant raw materials and does not contain a chemically synthesized mosquito repellent, the mosquito repellent time can be over 6 hours, the aroma is unique, and the perfume does not stimulate skin.
Description
Technical field
The invention provides a kind of mosquito-repellent perfume, particularly relating to a kind of take natural plant essential oils as the perfume of main active ingredient, belongs to daily chemical products technical field.
Background technology
Summer arrives, and the mosquito as one of " four pests " brings very large harm to the life of people.Drone sound is hovered in one's ear, disturbs one's sleep, and then has influence on new darg, studying and living.If unfortunate by mosquito bite, will ache and itch hard to bear, be on tenterhooks.More serious problem is that mosquito can propagate the diseases such as malaria, filaricide, epidemic encephalitis type B and dengue fever.Therefore, a good mosquito repellent product seems particularly important in summer.It can not only play good effectiveness, more importantly little to the health hazards of human body, is even free from side effects, simultaneously for environment without any pollution.Many people select, by the floral water having repelling effect, perfume, emulsion etc., mostly to use dimethyl phthalate and other some auxiliary elements of chemosynthesis, have certain stimulation and side effect to skin in these products.And infant is vulnerable to mosquito bite, the mosquito repellent product of these chemosynthesis compositions can to the healthy generation adverse influence of infant.And the repelling effect of traditional mosquito repellent product is also limited, can not accomplish that the time of anophelifuge or anophelifuge is completely too short.Also someone adopts ultrasonic mosquito dispelling, but this sound wave can produce adverse influence to the normal work of the electric equipment of surrounding, and sound wave is also can to some sensitive groups of surrounding, such as anemia of pregnant woman produces Health cost, and therefore its application also receives certain restriction.
Summary of the invention
The object of this invention is to provide a kind of perfume with repelling effect, increase the function of common perfume, fierce effect is not produced to skin.The technical scheme adopted is:
Comprise a preparation method for the mosquito-repellent perfume of natural plant essential oils, comprise the steps:
S1: by weight, get the stem and leaf 10 ~ 20 parts of Herba nepenthis, the stem and leaf 15 ~ 20 parts of Radix Buddlejae Butterflybush, the stem and leaf 5 ~ 10 parts of Flos Pelargonii, the stem and leaf 15 ~ 25 parts of Herba Menthae, after pulverizing, be placed in boiler, steam is led directly to from the boiler the bottom of a pan, steam pressure 3 ~ 5atm, distills, and the gas that distillation produces is collected in condensation, distillation time is 1 ~ 1.5h, after condensed fluid stratification, get the oil reservoir on upper strata, obtain blend of essential oils I;
S2: by weight, get Fructus Tritici aestivi 20 ~ 30 parts, Semen Maydis powder 10 ~ 15 parts, extracted by supercritical carbon dioxide extraction method, the technological parameter of extraction is: extracting pressure 10 ~ 15MPa, extraction temperature 40 ~ 50 DEG C, extraction time 2 ~ 3h; Then be separated, separating pressure is 4 ~ 6MPa, and separation temperature is 30 ~ 35 DEG C, obtains raffinate and blend of essential oils II;
S3: by weight, get Fructus Caricae 20 ~ 30 parts, the stem and leaf 20 ~ 30 parts of lindera thomsonii allen, the stem and leaf 10 ~ 20 parts of light Jasminum lanceolarium Roxb., the stem and leaf 5 ~ 10 parts of clover, the stem and leaf 10 ~ 20 parts of Radix Inulae, the stem and leaf 5 ~ 10 parts of Flos Matricariae chamomillae, the stem and leaf 10 ~ 20 parts of Ramulus et Folium Cotini Coggygiae, after cleaning, pulverize, be placed in boiler, steam is led directly to from the boiler the bottom of a pan, steam pressure 3 ~ 5atm, distill, the gas that distillation produces is collected in condensation, and distillation time is 1 ~ 1.5h, after condensed fluid stratification, get the oil reservoir on upper strata, obtain blend of essential oils III;
S4: radix valerianae 20 ~ 30 parts, Folium eucalypti globueli (Eucalyptus globulus Labill.) 20 ~ 30 parts, Folium Artemisiae Argyi 30 ~ 40 parts, after cleaning, be placed in boiler, lead directly to steam from the boiler the bottom of a pan, steam pressure 3 ~ 5atm, distill, the gas that distillation produces is collected in condensation, and distillation time is 1 ~ 1.5h, after condensed fluid stratification, get the oil reservoir on upper strata, obtain blend of essential oils IV;
S5: after blend of essential oils I, edible vegetable oil mixtures II, blend of essential oils III, blend of essential oils IV mix homogeneously, add 95 ~ 98% alcoholic solution (V/V) again, the weight adding alcoholic solution is 3 ~ 4 times of gross weight of blend of essential oils I, edible vegetable oil mixtures II, blend of essential oils III, blend of essential oils IV, slow stirring, leave standstill after 40 ~ 48 hours, proceed in hermetic container and carry out ageing 4 ~ 6 weeks, finally obtain finished product perfume.
Herba nepenthis, Radix Buddlejae Butterflybush, Flos Pelargonii, Herba Menthae have certain anophelifuge and fragrance effect.
Folium eucalypti globueli (Eucalyptus globulus Labill.) is the leaf of myrtle Eucalyptus globulus Labill.Toil, cool.Merit can dispelling wind to relieve the exterior syndrome; Heat-clearing and toxic substances removing; Phlegm-eliminiating and qi-regulating; Killing parasites for relieving itching.
Fructus Caricae is the fruit of Caricaceae plant Fructus Caricae.Sweet in the mouth; Property is put down.Merit can eliminating dampness and dredging channels; Removing toxic substances anthelmintic.
Radix valerianae is the root can taking from Valeriana officinalis var. latifolia (Valeriana officinalis Var.Latifolia Miq).Have wind dispelling, excitement, spasmolytic effect concurrently and there is tranquilizing by nourishing the heart, regulate the flow of vital energy, the effect such as promoting blood circulation and stopping pain.
Lindera thomsonii allen (lindera thomsonii allen), light Jasminum lanceolarium Roxb. (jasminum lanceolarium roxb), clover (asperulaodorata L.), Radix Inulae (inula helenium L.), Flos Matricariae chamomillae (matricaria chamomilla L.), Ramulus et Folium Cotini Coggygiae (cotinuscoggygria scopL) are natural perfume plant, may be used for the aromatic activity material as this perfume, its extract also has certain repelling effect.
In above-mentioned step S1, before vegetable material being carried out pulverize, being positioned over boiler, preferably be soaked in the sulfate liquor of 100 ~ 120 weight portions and soaked 2 ~ 3 hours, containing the zinc sulfate of 0.1 ~ 0.3mol/L and the aluminium potassium sulfate of 0.05 ~ 0.1mol/L in described sulfate liquor, after solid-liquid separation, vegetable material is taken out, then carries out the pulverizing described in step S1, mixing, distilation steps.The object done like this to destroy the cell of plant, makes the precipitation that effective ingredient is more, makes repelling effect better.
In above-mentioned step S2, after obtaining blend of essential oils II, to further purification processes, purifying technique is as follows: distilled in 130 ~ 150 DEG C of temperature ranges by blend of essential oils II, operating pressure is 0.01 ~ 0.05mmHg, obtains debris; Again debris is distilled in 200 ~ 220 DEG C of temperature ranges, fraction condensation is collected, obtains the blend of essential oils II refined.The object that above-mentioned step is done like this improves the limpid degree of outward appearance of final obtained perfume, occurs more precipitate in the process of prevention from decaying; In addition, because essential oil product obtains purification, the guard time of anophelifuge can also be extended, improve protected effect.
The preparation method of optimum of the present invention is:
S1: the stem and leaf 15kg getting Herba nepenthis, the stem and leaf 18kg of Radix Buddlejae Butterflybush, the stem and leaf 8kg of Flos Pelargonii, the stem and leaf 20kg of Herba Menthae, after pulverizing, mix homogeneously, to be soaked in the sulfate liquor with a 100kg 2 hours, containing the zinc sulfate of 0.1mol/L and the aluminium potassium sulfate of 0.05mol/L in described sulfate liquor, after solid-liquid separation, vegetable material is taken out, be placed in boiler, steam is led directly to from the boiler the bottom of a pan, steam pressure 4atm, distill, the gas that distillation produces is collected in condensation, distillation time is 1.2h, after condensed fluid stratification, get the oil reservoir on upper strata, obtain blend of essential oils I,
S2: get Fructus Tritici aestivi 25kg, Semen Maydis powder 12kg, mix homogeneously, extracted by supercritical carbon dioxide extraction method, the technological parameter of extraction is: extracting pressure 12MPa, extraction temperature 42 DEG C, extraction time 2.5h; Then be separated, separating pressure is 5MPa, separation temperature is 32 DEG C, obtain raffinate and blend of essential oils II, to the further purification processes of blend of essential oils II, purifying technique is as follows: distilled in 150 DEG C of temperature ranges by blend of essential oils II, operating pressure is 0.05mmHg, obtains debris; Again debris is distilled in 220 DEG C of temperature ranges, fraction condensation is collected, obtains the blend of essential oils II refined;
S3: get Fructus Caricae 25kg, the stem and leaf 25kg of lindera thomsonii allen, the stem and leaf 15kg of light Jasminum lanceolarium Roxb., the stem and leaf 8kg of clover, the stem and leaf 15kg of Radix Inulae, the stem and leaf 8kg of Flos Matricariae chamomillae, the stem and leaf 14kg of Ramulus et Folium Cotini Coggygiae, after cleaning, pulverizes, mix homogeneously, be placed in boiler, lead directly to steam from the boiler the bottom of a pan, steam pressure 4atm, distill, the gas that distillation produces is collected in condensation, and distillation time is 1.2h, after condensed fluid stratification, get the oil reservoir on upper strata, obtain blend of essential oils III;
S4: get radix valerianae 25kg, Folium eucalypti globueli (Eucalyptus globulus Labill.) 25kg, Folium Artemisiae Argyi 35kg, after cleaning, mix homogeneously, is placed in boiler, steam is led directly to from the boiler the bottom of a pan, steam pressure 4atm, distills, and the gas that distillation produces is collected in condensation, distillation time is 1.3h, after condensed fluid stratification, get the oil reservoir on upper strata, obtain blend of essential oils IV;
S5: after blend of essential oils I, refining edible vegetable oil mixtures II, blend of essential oils III, blend of essential oils IV mix homogeneously, add 95% alcoholic solution (V/V) again, the weight adding alcoholic solution is 3.5 times of gross weight of blend of essential oils I, edible vegetable oil mixtures II, blend of essential oils III, blend of essential oils IV, slow stirring, leave standstill after 45 hours, proceed in hermetic container and carry out ageing 5 weeks, finally obtain finished product perfume.
Beneficial effect
Mosquito-repellent perfume provided by the invention, have employed natural plant raw material, and not containing chemosynthesis anophelifuge, mosquito repellent time can reach more than 6 hours, and fragrance is unique, does not produce stimulation to skin.
Detailed description of the invention
Embodiment 1
S1: get the stem and leaf 10kg of Herba nepenthis, the stem and leaf 15kg of Radix Buddlejae Butterflybush, the stem and leaf 5kg of Flos Pelargonii, the stem and leaf 15kg of Herba Menthae, after pulverizing, be placed in boiler, lead directly to steam from the boiler the bottom of a pan, steam pressure 3atm, distill, the gas that distillation produces is collected in condensation, and distillation time is 1h, after condensed fluid stratification, get the oil reservoir on upper strata, obtain blend of essential oils I, weight is 1.1kg;
S2: get Fructus Tritici aestivi 20kg, Semen Maydis powder 10kg, extracted by supercritical carbon dioxide extraction method, the technological parameter of extraction is: extracting pressure 10MPa, extraction temperature 40 DEG C, extraction time 2h; Then be separated, separating pressure is 4MPa, and separation temperature is 30 DEG C, obtains raffinate and blend of essential oils II, and the weight of blend of essential oils II is 0.2kg;
S3: get Fructus Caricae 20kg, the stem and leaf 20kg of lindera thomsonii allen, the stem and leaf 10kg of light Jasminum lanceolarium Roxb., the stem and leaf 5kg of clover, the stem and leaf 10kg of Radix Inulae, the stem and leaf 5kg of Flos Matricariae chamomillae, the stem and leaf 10kg of Ramulus et Folium Cotini Coggygiae, after cleaning, pulverizes, be placed in boiler, lead directly to steam from the boiler the bottom of a pan, steam pressure 3atm, distills, the gas that distillation produces is collected in condensation, distillation time is 1h, after condensed fluid stratification, gets the oil reservoir on upper strata, obtain blend of essential oils III, weight is 1.5kg;
S4: get radix valerianae 20kg, Folium eucalypti globueli (Eucalyptus globulus Labill.) 20kg, Folium Artemisiae Argyi 30kg, after cleaning, be placed in boiler, lead directly to steam from the boiler the bottom of a pan, steam pressure 3atm, distill, the gas that distillation produces is collected in condensation, and distillation time is 1h, after condensed fluid stratification, get the oil reservoir on upper strata, obtain blend of essential oils IV, weight is 0.7kg;
S5: after blend of essential oils I, edible vegetable oil mixtures II, blend of essential oils III, blend of essential oils IV mix homogeneously, add 95% alcoholic solution (V/V) again, the weight adding alcoholic solution is 3 times of gross weight of blend of essential oils I, edible vegetable oil mixtures II, blend of essential oils III, blend of essential oils IV, slow stirring, leave standstill after 40 hours, proceed in hermetic container and carry out ageing 4 weeks, finally obtain finished product perfume.
Embodiment 2
S1: get the stem and leaf 15kg of Herba nepenthis, the stem and leaf 18kg of Radix Buddlejae Butterflybush, the stem and leaf 8kg of Flos Pelargonii, the stem and leaf 20kg of Herba Menthae, after pulverizing, mix homogeneously, be placed in boiler, lead directly to steam from the boiler the bottom of a pan, steam pressure 4atm, distills, the gas that distillation produces is collected in condensation, distillation time is 1.2h, after condensed fluid stratification, gets the oil reservoir on upper strata, obtain blend of essential oils I, weight is 1.2kg;
S2: get Fructus Tritici aestivi 25kg, Semen Maydis powder 12kg, mix homogeneously, extracted by supercritical carbon dioxide extraction method, the technological parameter of extraction is: extracting pressure 12MPa, extraction temperature 42 DEG C, extraction time 2.5h; Then be separated, separating pressure is 5MPa, and separation temperature is 32 DEG C, obtains raffinate and blend of essential oils II, and the weight of blend of essential oils II is 0.3kg;
S3: get Fructus Caricae 25kg, the stem and leaf 25kg of lindera thomsonii allen, the stem and leaf 15kg of light Jasminum lanceolarium Roxb., the stem and leaf 8kg of clover, the stem and leaf 15kg of Radix Inulae, the stem and leaf 8kg of Flos Matricariae chamomillae, the stem and leaf 14kg of Ramulus et Folium Cotini Coggygiae, after cleaning, pulverize, mix homogeneously, be placed in boiler, steam is led directly to from the boiler the bottom of a pan, steam pressure 4atm, distill, the gas that distillation produces is collected in condensation, and distillation time is 1.2h, after condensed fluid stratification, get the oil reservoir on upper strata, obtain blend of essential oils III, weight is 1.6kg;
S4: get radix valerianae 25kg, Folium eucalypti globueli (Eucalyptus globulus Labill.) 25kg, Folium Artemisiae Argyi 35kg, after cleaning, mix homogeneously, be placed in boiler, lead directly to steam from the boiler the bottom of a pan, steam pressure 4atm, distills, the gas that distillation produces is collected in condensation, distillation time is 1.3h, after condensed fluid stratification, gets the oil reservoir on upper strata, obtain blend of essential oils IV, weight is 0.8kg;
S5: after blend of essential oils I, edible vegetable oil mixtures II, blend of essential oils III, blend of essential oils IV mix homogeneously, add 95% alcoholic solution (V/V) again, the weight adding alcoholic solution is 3.5 times of gross weight of blend of essential oils I, edible vegetable oil mixtures II, blend of essential oils III, blend of essential oils IV, slow stirring, leave standstill after 45 hours, proceed in hermetic container and carry out ageing 5 weeks, finally obtain finished product perfume.
Embodiment 3
S1: get the stem and leaf 20kg of Herba nepenthis, the stem and leaf 20kg of Radix Buddlejae Butterflybush, the stem and leaf 10kg of Flos Pelargonii, the stem and leaf 25kg of Herba Menthae, after pulverizing, mix homogeneously, be placed in boiler, lead directly to steam from the boiler the bottom of a pan, steam pressure 5atm, distills, the gas that distillation produces is collected in condensation, distillation time is 1.5h, after condensed fluid stratification, gets the oil reservoir on upper strata, obtain blend of essential oils I, weight is 1.3kg;
S2: get Fructus Tritici aestivi 30kg, Semen Maydis powder 15kg, mix homogeneously, extracted by supercritical carbon dioxide extraction method, the technological parameter of extraction is: extracting pressure 15MPa, extraction temperature 50 DEG C, extraction time 3h; Then be separated, separating pressure is 6MPa, and separation temperature is 35 DEG C, obtains raffinate and blend of essential oils II, and the weight of blend of essential oils II is 0.3kg;
S3: get Fructus Caricae 30kg, the stem and leaf 30kg of lindera thomsonii allen, the stem and leaf 20kg of light Jasminum lanceolarium Roxb., the stem and leaf 10kg of clover, the stem and leaf 20kg of Radix Inulae, the stem and leaf 10kg of Flos Matricariae chamomillae, the stem and leaf 20kg of Ramulus et Folium Cotini Coggygiae, after cleaning, pulverize, mix homogeneously, be placed in boiler, steam is led directly to from the boiler the bottom of a pan, steam pressure 5atm, distill, the gas that distillation produces is collected in condensation, and distillation time is 1.5h, after condensed fluid stratification, get the oil reservoir on upper strata, obtain blend of essential oils III, weight is 1.8kg;
S4: get radix valerianae 30kg, Folium eucalypti globueli (Eucalyptus globulus Labill.) 30kg, Folium Artemisiae Argyi 40kg, after cleaning, mix homogeneously, be placed in boiler, lead directly to steam from the boiler the bottom of a pan, steam pressure 5atm, distills, the gas that distillation produces is collected in condensation, distillation time is 1.5h, after condensed fluid stratification, gets the oil reservoir on upper strata, obtain blend of essential oils IV, weight is 0.9kg;
S5: after blend of essential oils I, edible vegetable oil mixtures II, blend of essential oils III, blend of essential oils IV mix homogeneously, add 95% alcoholic solution (V/V) again, the weight adding alcoholic solution is 3 ~ 4 times of gross weight of blend of essential oils I, edible vegetable oil mixtures II, blend of essential oils III, blend of essential oils IV, slow stirring, leave standstill after 48 hours, proceed in hermetic container and carry out ageing 6 weeks, finally obtain finished product perfume.
Embodiment 4
Be with the difference of embodiment 2: in the middle of step S1, after the stem and leaf of the stem and leaf of the stem and leaf of Herba nepenthis, Radix Buddlejae Butterflybush, Flos Pelargonii, the stem and leaf of Herba Menthae are taken, to be soaked in the sulfate liquor with a 100kg 2 hours, containing the zinc sulfate of 0.1mol/L and the aluminium potassium sulfate of 0.05mol/L in described sulfate liquor, after solid-liquid separation, vegetable material is taken out, then puts into boiler.
Embodiment 5
Be with the difference of embodiment 2: in the middle of step S1, after the stem and leaf of the stem and leaf of the stem and leaf of Herba nepenthis, Radix Buddlejae Butterflybush, Flos Pelargonii, the stem and leaf of Herba Menthae are taken, to be soaked in the sulfate liquor with a 110kg 2.5 hours, containing the zinc sulfate of 0.2mol/L and the aluminium potassium sulfate of 0.08mol/L in described sulfate liquor, after solid-liquid separation, vegetable material is taken out
Embodiment 6
Be with the difference of embodiment 2: in the middle of step S1, after the stem and leaf of the stem and leaf of the stem and leaf of Herba nepenthis, Radix Buddlejae Butterflybush, Flos Pelargonii, the stem and leaf of Herba Menthae are taken, to be soaked in the sulfate liquor with a 120kg 3 hours, containing the zinc sulfate of 0.3mol/L and the aluminium potassium sulfate of 0.1mol/L in described sulfate liquor, after solid-liquid separation, vegetable material is taken out
Embodiment 7
Be with the difference of embodiment 4: in step s 2, after obtaining blend of essential oils II, to its further purification processes, purifying technique is as follows: distilled in 130 DEG C of temperature ranges by blend of essential oils II, operating pressure is 0.01mmHg, obtains debris; Debris distilled in 200 DEG C of temperature ranges, fraction condensation collected, obtain the blend of essential oils II refined, weight is 0.27kg again.
In step s 5, when taking alcoholic solution, be will calculate with the weight of the blend of essential oils II after refining.
Embodiment 8
Be with the difference of embodiment 4: in step s 2, after obtaining blend of essential oils II, to its further purification processes, purifying technique is as follows: distilled in 140 DEG C of temperature ranges by blend of essential oils II, operating pressure is 0.03mmHg, obtains debris; Debris distilled in 210 DEG C of temperature ranges, fraction condensation collected, obtain the blend of essential oils II refined, weight is 0.28kg again.
In step s 5, when taking alcoholic solution, be will calculate with the weight of the blend of essential oils II after refining.
Embodiment 9
Be with the difference of embodiment 4: in step s 2, after obtaining blend of essential oils II, to its further purification processes, purifying technique is as follows: distilled in 150 DEG C of temperature ranges by blend of essential oils II, operating pressure is 0.05mmHg, obtains debris; Debris distilled in 220 DEG C of temperature ranges, fraction condensation collected, obtain the blend of essential oils II refined, weight is 0.27kg again.
In step s 5, when taking alcoholic solution, be will calculate with the weight of the blend of essential oils II after refining.
Performance test
Test mosquito
Aedes albopictus (Aedes albopictus), is purchased from parasitic disease Shanghai Research Institute of Chinese Center for Disease Control (CDC), is national standard hygienic insecticide evaluating drug effect insecticide (GB/T17322.10-1998).Raised by Shanghai City institute of parasitic experimental insect receptacle and go down to posterity.Stricture of vagina yellow-fever mosquito grows into adult mosquito from egg development to be needed through larval phase (larva has 4 length of times) and two development and growth stages of pupa time, is complete metamorphosis.The rearing conditions of Aedes albopictus is: temperature 26 DEG C-28 DEG C, relative humidity 75%-85%, and the photoperiod (Light:Dark, L:D) is 12h/12h.Under this environmental condition, chosen by the worm's ovum of Aedes albopictus in the enamel tray filling dechlorination water (24h placed by tap water), after larvae hatch, every day adds a small amount of yeast powder.Along with instar larvae increases, the yeast powder be at every turn sprinkled into should increase in right amount.When larva pupates in a large number, pupa is transferred in bowl and put into mosquito cage, and in mosquito cage, put into the glass dish that glucose solution is housed.
Test mice
Kunming mice F1, is purchased from Shanghai institute of lab animals of the Chinese Academy of Sciences, is male entirely, weight 25g ± 2g, regular grade.Breed for laboratory animal breeding room of Shanghai institute of lab animals of the Chinese Academy of Sciences raises.
Anophelifuge test method
With reference to National Standard of the People's Republic of China, the method for indoor harmacological effect evaluation repellant (GB/T17355.10-1998) of agriculture chemical registration hygienic insecticide is tested
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.Wipe out after mouse web portion becomes mildewed, depilatory is applied to abdominal part, wipes with napkin after 5min, clean with tap water, dry with cotton balls.The depilation time should be not long, otherwise can destroy the skin of mice.Being fixed on by test mice folds up in the plastic plate of mouse, and abdominal part aims at the border circular areas (diameter 2.5cm) being put in hollow out, and extremity and tail adhesive tape are tightly wound around, and cover skin.Examination Mus is put into mosquito cage 2min, the examination worm coming to stop to fall is that attack is qualified more than 20 persons, and this Mus and this cage mosquito can be used for repellency test.
Anophelifuge is tested: with above-mentioned method process mice.Mice from (losing hair or feathers) the skin of abdomen that border circular areas (diameter 2.5cm) exposes, uniform application is for the mosquito-repellent perfume 20 μ L of examination, examination Mus is put into mosquito cage (having about 300 female mosquitos), observe 2min, record thorn stings the mosquito quantity of mice, put into mosquito cage at interval of 1h and observe whether have mosquito bite, observe 8h altogether, observe 2min at every turn.Each process establishes 3 mices to repeat, lining average, arranges the mice that abdominal part smears 20 μ L dehydrated alcohol and makes blank, observe the attacking ability of mosquito.Calculate the Effective Vate of Protection of each mosquito-repellent perfume, computing formula is as follows:
Effective Vate of Protection (%)=(contrast mosquito thorn sting number-be coated with mosquito thorn after quintessence oil to sting number)/contrast mosquito thorn stings number.
With mosquito-repellent perfume disclosed in patent CN102871931A in contrast.
Test data is as shown in table 1.
Table 1 protective rate test result
As can be seen from the table, the protective rate that mosquito-repellent perfume provided by the invention tests gained under 2h, 4h, 6h, 8h interval is all better than reference examples.The effect of the protective rate of the mosquito-repellent perfume of embodiment 4-embodiment 9 gained is also better than embodiment 1-embodiment 3 in addition; illustrate after plant material is used electrolyte solution soaking in advance; be conducive to breaking and the precipitation of organic principle of cell, the acquisition of organic principle in subsequent processing steps can be proposed.
The protective rate test result of embodiment 7-embodiment 9 is also better than embodiment 4-embodiment 6 slightly, illustrates after carrying out purification processes for essential oil product, also contributes to improving protected effect.Wherein, embodiment 9 is optimum.
Human trial
For examination insecticide: Aedes albopictus, the female adult mosquito of not sucking blood for the 4th day to the 5th day after sprouting wings;
Test condition: temperature 25 DEG C, relative humidity 65%;
Advanced pedestrian's body attack experimental test, growing × wide × high for putting into 300 examination worms in the mosquito cage of 40cm × 30cm × 30cm, expose 4cm × 4cm skin at the back of the hand, cover remainder.Stretched into by hands in mosquito cage and place 2min, unnecessary 30 persons of the examination worm coming to stop to fall are that attack is qualified, and the mosquito of this people and this cage can be used for repellency test;
Respectively draw the skin area of 5cm × 5cm at the both hands back of the people of 20 attack test passes, wherein a hands is blank, and another hands smears mosquito-repellent perfume to be measured, and dosage is 0.1ml/cm
2, expose 4cm × 4cm skin wherein, cover remainder.Smear 2h after mosquito-repellent perfume, hands is stretched into 2min in mosquito cage, observe and come to suck blood with or without mosquito, test in later every 2 hours once, as long as there is 1 mosquito to come to suck blood namely to be judged to repellant failure, carries out the test of 8 hours altogether.The effective protecting time (h) of record repellant;
The performance test data of table 2 embodiment 1 ~ embodiment 9 and reference examples
As can be seen from the table, the meansigma methods of the effective protecting time of the mosquito-repellent perfume of embodiment 1-embodiment 9, between 3-5 hour, is better than the meansigma methods 2 hours of reference examples.And the average effective guard time of embodiment 4-embodiment 6 is better than embodiment 1, illustrates after immersion treatment is carried out to plant material, contribute to the precipitation of its effective ingredient, can repelling effect be improved; In addition, the protective rate test result of embodiment 7-embodiment 9 is also better than embodiment 4-embodiment 6 slightly, illustrates after carrying out purification processes for essential oil product, also contributes to improving protected effect.Wherein, embodiment 9 is optimum.
Perfume turbidity is tested
Perfume turbidity is measured according to QB/T1858-2004 " perfume, GULONG water ".After perfume is completed ageing, take out and carry out turbidity test.
Table 3 perfume turbidity test result
As can be seen from the table, after quintessence oil is purified, contribute to the cloudiness reducing perfume.
This product is mainly applicable to, by the crowd of mosquito puzzlement, comprise consuming public, outdoor activities person, tour-pioneers, and the outdoor study personnel such as army, oil, geological prospecting, is especially applicable to child, Ms etc. and bears a pretty, delicate skin sensitive subjects.Appropriate this product of sprinkling, in baring skin surface, is smeared evenly.
Claims (1)
1. comprise the preparation method of the mosquito-repellent perfume of natural plant essential oils, it is characterized in that, comprise the steps:
S1: the stem and leaf 15kg getting Herba nepenthis, stem and leaf 18 kg of Radix Buddlejae Butterflybush, the stem and leaf 8kg of Flos Pelargonii, stem and leaf 20 kg of Herba Menthae, after pulverizing, mix homogeneously, to be soaked in the sulfate liquor with a 100kg 2 hours, containing the zinc sulfate of 0.1mol/L and the aluminium potassium sulfate of 0.05 mol/L in described sulfate liquor, after solid-liquid separation, vegetable material is taken out, be placed in boiler, steam is led directly to from the boiler the bottom of a pan, steam pressure 4atm, distill, the gas that distillation produces is collected in condensation, distillation time is 1.2h, after condensed fluid stratification, get the oil reservoir on upper strata, obtain blend of essential oils I,
S2: get Fructus Tritici aestivi 25kg, Semen Maydis powder 12kg, mix homogeneously, extracted by supercritical carbon dioxide extraction method, the technological parameter of extraction is: extracting pressure 12MPa, extraction temperature 42 DEG C, extraction time 2.5h; Then be separated, separating pressure is 5MPa, separation temperature is 32 DEG C, obtain raffinate and blend of essential oils II, to the further purification processes of blend of essential oils II, purifying technique is as follows: distilled in 150 DEG C of temperature ranges by blend of essential oils II, operating pressure is 0.05 mmHg, obtains debris; Again debris is distilled in 220 DEG C of temperature ranges, fraction condensation is collected, obtains the blend of essential oils II refined;
S3: get Fructus Caricae 25 kg, stem and leaf 25 kg of lindera thomsonii allen, stem and leaf 15 kg of light Jasminum lanceolarium Roxb., clover (
asperula odorata L.) stem and leaf 8kg, the stem and leaf 15kg of Radix Inulae, the stem and leaf 8kg of Flos Matricariae chamomillae, stem and leaf 14 kg of Ramulus et Folium Cotini Coggygiae, clean after, pulverize, mix homogeneously, be placed in boiler, lead directly to steam from the boiler the bottom of a pan, steam pressure 4atm, distill, the gas that distillation produces is collected in condensation, and distillation time is 1.2h, after condensed fluid stratification, get the oil reservoir on upper strata, obtain blend of essential oils III;
S4: get radix valerianae 25 kg, Folium eucalypti globueli (Eucalyptus globulus Labill.) 25 kg, Folium Artemisiae Argyi 35 kg, after cleaning, mix homogeneously, is placed in boiler, steam is led directly to from the boiler the bottom of a pan, steam pressure 4atm, distills, and the gas that distillation produces is collected in condensation, distillation time is 1.3h, after condensed fluid stratification, get the oil reservoir on upper strata, obtain blend of essential oils IV;
S5: after blend of essential oils I, refining blend of essential oils II, blend of essential oils III, blend of essential oils IV mix homogeneously, add 95% alcoholic solution (V/V) again, the weight adding alcoholic solution is 3.5 times of gross weight of blend of essential oils I, refining blend of essential oils II, blend of essential oils III, blend of essential oils IV, slow stirring, leave standstill after 45 hours, proceed in hermetic container and carry out ageing 5 weeks, finally obtain finished product perfume.
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| CN105411840A (en) * | 2014-09-23 | 2016-03-23 | 南阳师范学院 | Microwave moxibustion instrument, preparing method thereof and use method thereof |
| CN106176371A (en) * | 2016-07-29 | 2016-12-07 | 金玛瑙香水（明光）有限公司 | A kind of natural skin care perfume and preparation method thereof |
| CN109010204A (en) * | 2018-08-06 | 2018-12-18 | 大连民族大学 | A kind of delicate fragrance pawpaw perfume |
| CN109439434A (en) * | 2018-11-22 | 2019-03-08 | 河南农业大学 | The extracting method of smoke tree essence |
| CN109381354A (en) * | 2018-11-26 | 2019-02-26 | 金玛瑙香水（明光）有限公司 | A kind of Longaacting fragrance-aretaining mosquito-repellent perfume |
| CN109757531A (en) * | 2019-02-18 | 2019-05-17 | 成都善禾天成生物科技有限公司 | Mosquito repellent liquid and preparation method thereof |
| CN115737509B (en) * | 2023-01-10 | 2023-04-21 | 广州市雪蕾化妆品有限公司 | Plant-based perfume and preparation method thereof |
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