CN104873420A

CN104873420A - Preparation method of natural mosquito repellent

Info

Publication number: CN104873420A
Application number: CN201510259179.7A
Authority: CN
Inventors: 李苏杨; 李文遐; 徐勤霞
Original assignee: Suzhou Bec Biological Technology Co Ltd
Current assignee: Suzhou Bec Biological Technology Co Ltd
Priority date: 2015-05-20
Filing date: 2015-05-20
Publication date: 2015-09-02

Abstract

The invention discloses a preparation method of a natural mosquito repellent. The method comprises the following steps: firstly, crushing monkshood, radix aconiti agrestis, radix angelicae pubescentis, rhizoma nardostachyos, nux vomica and radix angelicae into crude powder, and dipping with ethanol, wherein the percolating speed is 3-5mL/min, collecting percolate, extracting with diethyl ether, and carrying out vacuum recovery on an extract liquid to obtain an extract liquid I; mixing honeysuckle flower, liquorice, agastache rugosus, rhizoma atractylodis, clove and scutellaria baicalensis, and extracting with a supercritical carbon dioxide extraction method to obtain an extract liquid II; and mixing the extract liquid I with the extract liquid II, adding a 95v/v% ethanol solution, stirring, standing for 45 hours and then transferring into an airtight container, aging for 5 weeks, so as to obtain the mosquito repellent. According to the natural mosquito repellent disclosed by the invention, natural plant raw materials are adopted, so that a chemical synthetic insect repellent is not contained; the mosquito-repellent time is not less than 6 hours; and the natural mosquito repellent is unique in fragrance and free of thrill to skin.

Description

A kind of preparation method of natural anophelifuge agent

Technical field

The invention belongs to daily chemical products technical field, be specifically related to a kind of preparation method of natural anophelifuge agent.

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 the invention is to overcome the deficiencies in the prior art and the preparation method that a kind of natural anophelifuge agent is provided, this natural anophelifuge agent have employed natural plant raw material, and not containing chemosynthesis anophelifuge, mosquito repellent time can reach more than 6 hours, fragrance is unique, does not produce stimulation to skin.

A preparation method for natural anophelifuge agent, comprises the following steps:

Step 1, with parts by weight, get Radix Aconiti 4 ~ 7 parts, Radix Aconiti Kusnezoffii 3 ~ 8 parts, Radix Angelicae Pubescentis 2 ~ 6 parts, Radix Et Rhizoma Nardostachyos 1 ~ 5 part, Semen Strychni 3 ~ 8 parts, the Radix Angelicae Dahuricae 1 ~ 5 part, be ground into coarse powder, first use alcohol dipping, percolation speed is 3 ~ 5mL/min, collect percolate, reclaim ethanol and obtain concentrated solution, then use extracted with diethyl ether, gained extract reclaim under reduced pressure, obtains extracting solution I;

Step 2, with parts by weight, extracting honeysuckle 2 ~ 6 parts, 3 ~ 7 parts, Radix Glycyrrhizae, Herba Pogostemonis 2 ~ 6 parts, Rhizoma Atractylodis 1 ~ 5 part, Flos Caryophylli 4 ~ 7 parts, Radix Scutellariae 1 ~ 5 part, mix homogeneously, is first extracted by supercritical carbon dioxide extraction method, extracting pressure 12MPa, extraction temperature 42 DEG C, extraction time 2.5h, be separated again, separating pressure 6MPa, separation temperature is 40 DEG C, obtains extracting solution II;

Step 3, mixes step 1 gained extracting solution I and step 2 gained extracting solution II, adds 95v/v% alcoholic solution, stirs, and leaves standstill after 45 hours, proceeds in hermetic container and carry out ageing 5 weeks, obtain anophelifuge.

As the further improvement of foregoing invention, with 95v/v% alcohol dipping coarse powder 24h in step 1.

As the further improvement of foregoing invention, in step 1, gained concentrated solution relative density is 1.20 ~ 1.25.

As the further improvement of foregoing invention, in step 1, gained extract is 60 DEG C of water-bath reclaim under reduced pressure.

As the further improvement of foregoing invention, the weight adding alcoholic solution in step 3 is 3.5 times of the gross weight of extracting solution I and extracting solution II.

Natural anophelifuge agent of the present 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

Step 1, with parts by weight, get Radix Aconiti 4 parts, Radix Aconiti Kusnezoffii 3 parts, Radix Angelicae Pubescentis 2 parts, Radix Et Rhizoma Nardostachyos 1 part, Semen Strychni 3 parts, the Radix Angelicae Dahuricae 1 part, be ground into coarse powder, first use 95v/v% alcohol dipping coarse powder 24h, percolation speed is 3mL/min, collect percolate, reclaim ethanol and obtain concentrated solution, then use extracted with diethyl ether, gained extract, 60 DEG C of water-bath reclaim under reduced pressure, obtains extracting solution I;

Step 2, with parts by weight, extracting honeysuckle 2 parts, 3 parts, Radix Glycyrrhizae, Herba Pogostemonis 2 parts, Rhizoma Atractylodis 1 part, Flos Caryophylli 4 parts, Radix Scutellariae 1 part, mix homogeneously, is first extracted by supercritical carbon dioxide extraction method, extracting pressure 12MPa, extraction temperature 42 DEG C, extraction time 2.5h, be separated again, separating pressure 6MPa, separation temperature is 40 DEG C, obtains extracting solution II;

Step 3, mixes step 1 gained extracting solution I and step 2 gained extracting solution II, adds 95v/v% alcoholic solution, the weight adding alcoholic solution is 3.5 times of the gross weight of extracting solution I and extracting solution II, stirs, and leaves standstill after 45 hours, proceed in hermetic container and carry out ageing 5 weeks, obtain anophelifuge.

Embodiment 2

Step 1, with parts by weight, get Radix Aconiti 6 parts, Radix Aconiti Kusnezoffii 5 parts, Radix Angelicae Pubescentis 3 parts, Radix Et Rhizoma Nardostachyos 4 parts, Semen Strychni 6 parts, the Radix Angelicae Dahuricae 2 parts, be ground into coarse powder, first use 95v/v% alcohol dipping coarse powder 24h, percolation speed is 4mL/min, collect percolate, reclaim ethanol and obtain concentrated solution, then use extracted with diethyl ether, gained extract, 60 DEG C of water-bath reclaim under reduced pressure, obtains extracting solution I;

Step 2, with parts by weight, extracting honeysuckle 5 parts, 4 parts, Radix Glycyrrhizae, Herba Pogostemonis 3 parts, Rhizoma Atractylodis 2 parts, Flos Caryophylli 5 parts, Radix Scutellariae 4 parts, mix homogeneously, is first extracted by supercritical carbon dioxide extraction method, extracting pressure 12MPa, extraction temperature 42 DEG C, extraction time 2.5h, be separated again, separating pressure 6MPa, separation temperature is 40 DEG C, obtains extracting solution II;

Embodiment 3

Step 1, with parts by weight, get Radix Aconiti 7 parts, Radix Aconiti Kusnezoffii 8 parts, Radix Angelicae Pubescentis 6 parts, Radix Et Rhizoma Nardostachyos 5 parts, Semen Strychni 8 parts, the Radix Angelicae Dahuricae 5 parts, be ground into coarse powder, first use 95v/v% alcohol dipping coarse powder 24h, percolation speed is 5mL/min, collect percolate, reclaim ethanol and obtain concentrated solution, then use extracted with diethyl ether, gained extract, 60 DEG C of water-bath reclaim under reduced pressure, obtains extracting solution I;

Step 2, with parts by weight, extracting honeysuckle 6 parts, 7 parts, Radix Glycyrrhizae, Herba Pogostemonis 6 parts, Rhizoma Atractylodis 5 parts, Flos Caryophylli 7 parts, Radix Scutellariae 5 parts, mix homogeneously, is first extracted by supercritical carbon dioxide extraction method, extracting pressure 12MPa, extraction temperature 42 DEG C, extraction time 2.5h, be separated again, separating pressure 6MPa, separation temperature is 40 DEG C, obtains extracting solution II;

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/T 17322.10-1998).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.

Test data is as shown in the table.

Protective rate test result

Test parameter	Embodiment 1	Embodiment 2	Embodiment 3	Commercially available prod
					2h protective rate %	100％	100％	100％	100％
4h protective rate %	61％	62％	63％	55％
					6h protective rate %	34％	33％	32％	26％
8h protective rate %	15％	13％	14％	2％

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 commercially available prod.

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; Result is as shown in the table.

Tester	Embodiment 1	Embodiment 2	Embodiment 3	Commercially available prod
					1	2	2	4	2

2	2	2	2	2
					3	4	2	2	2
4	2	2	2	2
					5	4	4	2	2
6	2	4	2	2
					7	4	4	4	2
8	4	2	4	2
					9	2	4	2	0
10	2	4	4	2
					11	4	4	4	2
12	4	4	4	2
					13	4	2	4	2
14	4	2	2	2
					15	4	4	4	4
16	4	4	4	2
					17	2	4	4	2
18	2	4	4	0
					19	2	2	2	2
20	4	4	4	4
					Meansigma methods	3.1	3.2	3.2	2

As can be seen from the table, the meansigma methods of the effective protecting time of the mosquito-repellent perfume of embodiment 1-embodiment 3, between 3-5 hour, is better than the meansigma methods 2 hours of commercially available prod.

Claims

1. a preparation method for natural anophelifuge agent, is characterized in that: comprise the following steps:

2. the preparation method of natural anophelifuge agent according to claim 1, is characterized in that: with 95 v/v % alcohol dipping coarse powder 24h in step 1.

3. the preparation method of natural anophelifuge agent according to claim 1, is characterized in that: in step 1, gained concentrated solution relative density is 1.20 ~ 1.25.

4. the preparation method of natural anophelifuge agent according to claim 1, is characterized in that: in step 1, gained extract is 60 DEG C of water-bath reclaim under reduced pressure.

5. the preparation method of natural anophelifuge agent according to claim 1, is characterized in that: the weight adding alcoholic solution in step 3 is 3.5 times of the gross weight of extracting solution I and extracting solution II.