CN102949297A

CN102949297A - Mosquito repellent gel and preparation method thereof

Info

Publication number: CN102949297A
Application number: CN2012101958061A
Authority: CN
Inventors: 王宗德; 陈金珠; 范国荣; 蔡美萍; 陈尚钘
Original assignee: Jiangxi Agricultural University
Current assignee: Jiangxi Agricultural University
Priority date: 2012-06-14
Filing date: 2012-06-14
Publication date: 2013-03-06

Abstract

The invention discloses the preparation of a mosquito repellent gel. The mosquito repellent gel is characterized by consisting of a mosquito repellent effective ingredient and a gel carrier; the gel ingredient consists of the following components in percentage by mass: 5-20% of mosquito repellent agent (R2), 0.5-1.5% of base material, 0.8-2% of neutralization alkali, 5-16% of moisturizing agent, 0.2-0.4% of preservative, an appropriate amount of essence and the balance of de-ionized water; and the total percentage by mass is 100%. The mosquito repellent gel is easy to coat, has no irritation for the skin and has good mosquito repellent activity. The repellent time of the R2 gel with a concentration of 10% for three mosquito varieties comprising Aedesalbopictus, Culex pipiens quinquefasciatus and Culex pipiens can respectively reach the international grade B. The R2 gel further enriches the dosage form varieties of the terpene mosquito repellents and promotes the development of the plant repellents.

Description

Anophelifuge gel and preparation method

Technical field

The present invention relates to a kind of gelinite anophelifuge, especially the gelinite anophelifuge take botanical components as active component is easy to use, safety and comfort, at home suitable and field usage.

Technical background

Insect repellent occupies main status in insect control, many insect vectors sting to suck blood by thorn and spread disease, though go back some hematophagus without dissemination, serious to people's harassing and wrecking, also can cause dermatosis.People, the especially officers and men of army of life in the environment such as forest, grassland and wilderness, work and tourism are when on duty and training, using repellant is that (fiber crops are firm for important preventive means, Deng. Chinese hygienic biocide medical instruments, 2004,10 (6): 349.).

Diethyltoluamide (DEET) is a kind of repellant commonly used, but find successively its some shortcomings recently, what cause relatively that people pay close attention to is some problems of finding aspect toxicology, (the Qiu HC such as neurological symptom can occur such as irritated, the long-term or a large amount of use of child Et al.Journal of the American Mosquito Control Association, 1998,14 (1): 12-27.).

The repellent effect of many terpenoid repellents is better, mostly has armaticity, toxicity is low, zest is little, to human body and environmentally friendly, uses safety.Therefore, terpenoid repellents more and more cause people research and development interest (Wang Zongde, etc. Chinese hygienic biocide medical instruments, 2004,10 (1): 77-80.).

Hydroxycitronellal 1,2-PD acetal (R2) is a kind of terpenoid repellents, belongs to the micro-virus kind pesticide, rat acute per os LD ₅₀Female is 5840 mg/kg(95 % fiducial limits: 4300 ~ 7940), male is 6810 mg/kg.Alcoholic solution when concentration is 20 % to Aedes albopictus ( Aedes albopictus) repellent times 5 ~ 6 h, when concentration is 10 % and 20 % to Anopheles sinensis ( Anopheles sinensis) the repellent time be respectively 4.5 ~ 5 h and 5 ~ 6 h, all above B level national standard, when concentration is 20 % to culex pipiens pallens ( Culex pipiens) the repellent time be that 6.5 ~ 7 h surpass GB A level (Wang Zongde waits .CN 101889572 A, 2010; Yi Tingxin, etc. Chinese hygienic biocide medical instruments, 2010,16 (2): 120-122; Wang Zongde, etc. insecticide journal, 2010,53 (11): 1241-1247.).

The dosage form of past terpenoid repellents is relatively less, is tincture and unguentum substantially, and dosage form developed to some extent in recent years, some new dosage forms occurred, mainly comprises polymer formulations, solid preparation, microcapsule formulation.

At present, the key problem of repellant dosage form research is how to reduce volatilization and skin absorption, prolongs guard time, and wherein using slow releasing agent is a kind of very effective method.Slow releasing agent can get up anophelifuge activity composition temporary storage, after make again its slow release out, reach the purpose that reduces loss, prolongs the repellent time.The physics slow releasing agent is that active substance and polymer are blended together one, the chemical slow release agent is that active substance and polymer are combined by forming chemical bonded refractory, and (history is defended the country, etc. the anti-system of medical faunae to reach slow releasing function, 1998,14 (6): 4-6.).

Summary of the invention

The object of the invention is to study the slow-releasing gel used of a kind of repellant, namely adopting macromolecular compound is carrier, with anophelifuge activity composition R2 Uniform Dispersion therein, make the slow release formulation with prolongation repellent time, and the preparation method of this anophelifuge gel is provided.

Anophelifuge gel of the present invention is made of anophelifuge effective ingredient and gel carrier, gel agent composition is made of the component of following mass percent: mosquito-repellent (R2) 5 % ~ 20 %, substrate 0.5 % ~ 1.5 %, neutralization bases 0.8 % ~ 2 %, wetting agent 5 % ~ 16 %, antiseptic 0.2 % ~ 0.4 %, an amount of essence, all the other are deionized water, amount to 100 %.

Above-mentioned mosquito-repellent (R2) is hydroxycitronellal 1,2-PD acetal, is a kind of plant source terpenoid repellents; Described gel-type vehicle is Acritamer 940 aqueous gel substrate; Described neutralization bases is triethanolamine; Described wetting agent is 1,2 – propylene glycol, glycerol and hyaluronate sodium, is that cosmetic industry uses more widely wetting agent; Described antiseptic is parabens, is to use maximum, safer antiseptic in the present cosmetic industry.

Among the present invention, the employing Acritamer 940 is gel-type vehicle, and is more stable in acid or alkali environment because of it, but unstable in the presence of ion, and the used water of used the present invention is deionized water.Contain 52%～68% carboxyl in the Acritamer 940 molecule, the pH value of the carbomer aqueous solution of 1 % is 2.5～3.0, and GB regulation toiletries product acid base number is neutral, so add the neutralization bases neutralization, triethanolamine is the neutralization bases of relatively commonly using, and consumption generally is 1.0 ~ 1.2 times of carbomer concentration.

The preparation method of anophelifuge gel of the present invention is comprised of following steps:

(1) the Acritamer 940 gradation is joined in an amount of deionized water, stir with homogenizer, place after stirring and spend the night, make its abundant swelling, at room temperature operation.

(2) slowly add glycerol, hyaluronate sodium and 1,2-PD in the gel solution for preparing, the limit edged stirs.

(3) slowly drip again an amount of triethanolamine, antiseptic and spice, fully mixing.

(4) add again R2, and fully stir.

(5) replenish deionized water to the gel of desired concn, fully stir evenly and get final product.

The stability study of R2 gel.

Concrete research contents: prepare three batches of gels, a batch sample seals in the calorstat that is placed on (54 ± 2) ℃, preserves 1 month; Another batch sample is put into the refrigerator of (10 ± 1) ℃ and was preserved 1 month, investigates the centrifugal stability of gel under high temperature, cryogenic conditions and pH, effective ingredient Changing Pattern.The 3rd batch is placed on temperature (25 ± 2) ℃, relative humidity for preserving 6 months under (60 ± 10) % condition, and measures the anophelifuge activity to Aedes albopictus.

The result is presented in hot test and the low-temperature test, and having good stability of gel is clear gel still, without lamination.Between 6.5 ~ 8, active constituent content is without obvious fluctuation substantially for pH value.Preserve after 6 months, still have preferably repellent activity, the repellent time reaches more than 4.5 h, reaches GB B level.

Anophelifuge gel of the present invention easily is coated with exhibition, and to the skin nonirritant, anophelifuge activity is good, concentration be 10 % the R2 gel to Aedes albopictus ( Aedes albopictus), Culex quinquefasciatus ( Culex pipiens quinquefasciatus), culex pipiens pallens ( Culex pipiens) repellent time of three kinds of mosquito kinds reaches respectively 4 h, 5 h, 5 h, all reaches GB B level.The R2 gel has further enriched the dosage form kind of terpenoid repellents, promotes the development of plant source repellant.

The specific embodiment

Embodiment 1:

Get the R2 that mass percent is 10 %; The Acritamer 940 of 1 %; The triethanolamine of 1 %; The hyaluronate sodium of the glycerol of the 1,2-PD of 5 %, 5 %, 0.05 %; 0.08 the propylparaben of the methyl hydroxybenzoate of %, 0.12 %; 0.5 the essence of %; Surplus is deionized water.With carbomer joining in the deionized water slowly, fully stir with homogenizer, place after stirring and spend the night, make its abundant swelling.Add 1,2-PD, glycerol, hyaluronate sodium again in swelling solution, the limit edged stirs, and adds triethanolamine, antiseptic again, adds at last R2, both fully stirs evenly to get.

Embodiment 2:

Get the R2 that mass percent is 12.5 %; The Acritamer 940 of 1 %; 1.2 the triethanolamine of %; The hyaluronate sodium of the glycerol of the 1,2-PD of 10 %, 5 %, 0.1 %; 0.12 the propylparaben of the methyl hydroxybenzoate of %, 0.18 %; 0.3 the essence of %; Surplus is deionized water.Make first the carbomer gel carrier by same procedure, again R2 is dispersed on the carrier, both.

Embodiment 3:

Mass percent be 10 % and 12.5 % the R2 gel to Aedes albopictus ( Aedes albopictus) indoor repellency test.

Method with reference to standard GB/T/T 13917.9-2009 is carried out.

Indoor conditions: temperature (26 ± 1) ℃, relative humidity (65 ± 10) %.

Mosquito cage: long 400 mm, wide 300 mm, high 300 mm.

(men and women half and half to select 4 and the qualified tester of above attack, and before the test and the duration of test tea or coffee of should not drinking, should not use and contain the essence class and get product), wherein a back of the hand is blank, each contrast hands is done first the contrast test, the examination worm that attack is qualified can continue test, and examination worm attack is defective then need be changed qualified examination worm and test.Another the back of the hand is by 1.5 mg/cm ²Dosage evenly smear gel, and expose 4 cm of both hands * 4cm skin, other parts are tightly covered.Hands is stretched into 2 min in the qualified mosquito cage of attack, make gel and lost efficacy as long as have a mosquito to come to suck blood namely to declare.The effective protecting time (h) of record gel, and get its meansigma methods (keeping 2 decimals) as the effective protecting time (h) of this medicament, result such as table 1.

Table 1 R2 gel is to the repellent effect of Aedes albopictus

Annotate: "+" expression has a mosquito bite to judge that namely repellant lost efficacy, and "-" represents without mosquito bite

When the working concentration of R2 anophelifuge gel is 10 % and 12.5 %, the effective repellent of the Aedes albopictus time reached is respectively 4 h and 4.5 h, the result all reaches the B grade standard that GB/T 13917.9-2009 estimates.

Embodiment 4:

Mass percent be 10 % and 12.5 % the R2 gel to Culex quinquefasciatus ( Culex pipiens quinquefasciatus) indoor repellency test.

Concrete assay method is the same.Because Culex quinquefasciatus is the mosquito kind of sucking blood night, so indoor repellency test must carry out in night or the artificial dark surrounds that arranges.Record effective repellent time, result such as table 2.

Table 2 R2 gel is to the repellent effect of Culex quinquefasciatus

When the working concentration of R2 anophelifuge gel is 10 %, the effective repellent of the Culex quinquefasciatus time is reached 5 h, reach national B grade standard.When working concentration was 12.5 %, guard time reached 6 h, reached national A grade standard.

Embodiment 5:

Mass percent be 10 % and 12.5 % the R2 gel to culex pipiens pallens ( Culex pipiens) indoor repellency test.

Concrete assay method is the same.Because culex pipiens pallens also is the mosquito kind of sucking blood night, so indoor repellency test must carry out in night or the artificial dark surrounds that arranges.Record effective repellent time, result such as table 3.

Table 3 R2 gel is to the repellent effect of culex pipiens pallens

When the working concentration of R2 anophelifuge gel is 10 %, the effective repellent of the culex pipiens pallens time is reached 5 h, reach national B grade standard.When working concentration was 12.5 %, guard time reached 6 h, reached national A grade standard.

Embodiment 6:

R2 gel anophelifuge activity effect duration is measured: be preservation 6 months under (60 ± 10) % condition with the R2 gel of example 1 and example 2 preparations at temperature (25 ± 2) ℃, relative humidity, measured it to the anophelifuge activity of Aedes albopictus at 1 month, 3 months, 6 months respectively.

Concrete assay method is the same, result such as table 4.

The mensuration of table 4 R2 anophelifuge gel effect duration

After the result showed 6 months, concentration was that the gel effective protecting time of 10 %, 12.5 % is respectively 4 h, 4.5 h, reaches national B grade standard, has preferably repellent activity, illustrated that R2 gel effect duration reached more than half a year.

Claims

1. the preparation of an anophelifuge gel, it is characterized in that being consisted of by anophelifuge effective ingredient and gel carrier, gel agent composition is made of the component of following mass percent: mosquito-repellent (R2) 5 % ~ 20 %, substrate 0.5 % ~ 1.5 %, neutralization bases 0.8 % ~ 2 %, wetting agent 5 % ~ 16 %, antiseptic 0.2 % ~ 0.4 %, an amount of essence, all the other are deionized water, amount to 100 %.

2. above-mentioned mosquito-repellent (R2) is hydroxycitronellal 1,2-PD acetal.

3. according to anophelifuge gel claimed in claim 1, it is characterized in that:

Described mosquito component is that purity is the hydroxycitronellal 1,2-PD acetal of 92.7 %;

The substrate of described gel is the Acritamer 940 gel-type vehicle;

Described neutralization bases is triethanolamine.

4. according to anophelifuge gel claimed in claim 1, it is characterized in that described wetting agent is 1,2-PD, glycerol and hyaluronate sodium, the percentage ratio that its each component accounts for gross mass is:

1,2-PD 5 % ~ 10 %

Glycerol 0 ~ 5 %

Hyaluronate sodium 0 ~ 1 %

According to anophelifuge gel claimed in claim 1, it is characterized in that described antiseptic is compound preservative, its component constitutes:

Methyl hydroxybenzoate 0.08 % ~ 0.16 %

Propylparaben 0.12 % ~ 0.24 %.

5. according to the preparation method of anophelifuge gel claimed in claim 1, it is characterized in that being formed by following steps:

The Acritamer 940 gradation is joined in an amount of deionized water, stir with homogenizer, place after stirring and spend the night, make its abundant swelling, at room temperature operation;

Slowly add glycerol, hyaluronate sodium and 1,2-PD in the gel solution for preparing, the limit edged stirs;

Slowly drip again an amount of triethanolamine, antiseptic and spice, fully mixing;

Add again R2, and fully stir;

Replenish deionized water to the gel of desired concn, fully stir evenly and get final product.