CN104068062A - Chloramine tetramethrin emulsion in water for repelling and killing mosquitoes and flies and preparation method thereof - Google Patents
Chloramine tetramethrin emulsion in water for repelling and killing mosquitoes and flies and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a chloramine pyrethrins O/W type emulsion in water for repelling and killing mosquitoes and flies and a preparation method thereof. An emulsion in water of 1000 mL comprises raw materials by weight as follows: 3 to 7 g of tetramethrin, 13 to 17 g of chloramine tetramethrin, 48 to 52 mL of Tween-80, 18 to 22 mL of Span-80, and 3 to 7 g of milk flavor. The chloramine pyrethrins emulsion in water is a green environmental-friendly preparation, which contains no organic solvent, is low in production cost, prominent in repelling and killing mosquitoes and flies, simple in preparation technology, stable in quality, safe to people and livestock, convenient for use, reliable in effect, and suitable for places such as households, public places, and livestock farms.
Description
Technical field
The invention belongs to technical field of medicine, be specifically related to chlorine tetramethrin aqueous emulsion of a kind of repelling and killing bugs and preparation method thereof.
Background technology
The repelling and killing bugs medicine that China market is sold is at present still taking missible oil formulation as main, because missible oil excitant is large, solvent is inflammable and contaminated environment, because new drug development need to drop into substantial contribution, under current economic form, many companies turn to emphasis the exploitation of novel form simultaneously.Aqueous emulsion (Emulsion in water, EW) be the class emulsion dosage form (being O/W type) taking water as dispersion medium, particle diameter is between 0.1～50.0 μ m, outward appearance is milky, continuous phase is water, in formula, consumption of organic solvent is less or containing organic solvent, compared with traditional veterinary drug formulation---and it is little, nonflammable and use the advantages such as safety that missible oil has environmental pollution.Therefore, the research and development of domestic repelling and killing bugs aqueous emulsion become focus.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art, and chlorine tetramethrin aqueous emulsion of a kind of repelling and killing bugs and preparation method thereof is provided, and to improve its repelling and killing bugs effect, reduces environmental pollution.
In order to achieve the above object, technical scheme provided by the invention is:
The chlorine tetramethrin aqueous emulsion of described repelling and killing bugs, is characterized in that, aqueous emulsion is made up of the raw material of following weight described in 1000mL:
Preferably, described in 1000mL, in aqueous emulsion, can also contain 3～7g, preferably 5g milk flavour.
Preferably, the raw material composition that contains following weight in aqueous emulsion described in 1000mL:
In 1000mL aqueous emulsion, the preparation method of above-mentioned chlorine tetramethrin aqueous emulsion comprises the steps:
(1) take tetramethrin and permethrin by the weight described in claims 1 to 3 any one, under 80 DEG C～100 DEG C conditions, dissolve tetramethrin with permethrin, obtain A liquid;
(2) take Tween 80 and Si Ban 80 by the weight described in claims 1 to 3 any one, mix, obtain B liquid;
(3) A liquid and B liquid are uniformly mixed under 40～60 DEG C of conditions, obtain C liquid;
(4) to the water that adds 40～60 DEG C in C liquid, obtain white emulsion, then add water to 1000mL, obtain chlorine tetramethrin aqueous emulsion.
Preferably, can also in step (4) gained white emulsion, add milk flavour solution, then add water to 1000mL.
Preferably, described step (1) is dissolved tetramethrin with permethrin under 90 DEG C of conditions;
Preferably, step (3) is under 55 DEG C of conditions, to mix A liquid and B liquid.
The present invention obtains finished product by tetramethrin, permethrin, Tween 80 (Tween-80), 80 (Span-80) of class of department, milk flavour etc. through proper proportion dissolving, mixing, stirring, packing, is applied to repelling and killing bugs.Its innovation is:
1, the present invention mixes surfactant Tween 80 to be applied in chlorine tetramethrin aqueous emulsion with class of department 80 first, and show that the two best configuration proportion in this aqueous emulsion is 5:1.The stability of emulsion is a topic of quite being disputed in emulsion always; preparing the oily exactly breast separation of the most incidental problem of emulsion is layering; and the improper use of surfactant is layering soon after often can making emulsion form or to form, so the selection of surfactant and compatibility thereof are the key technologies of this test.Tween 80, class of department 80 are all nonionic surface active agent and emulsifier, Tween 80 is O/W type emulsifier, nontoxic non-stimulated, difficult combustion, water-soluble, have that good emulsification is wetting, dispersion and a permeance property, class of department 80 is W/O (Water-In-Oil) type emulsifier, for non-water-soluble emulsifier, these two kinds of emulsifier all have application more widely clinically.Through By consulting literatures and clinical testing, confirm that these two kinds of surfactants mix in proportion result of use and are better than single surfactant, and the two mixed proportion and its hydrophilic lipophilic balance (HLB value) are closely related, when making HLB value, the two mixed proportion is positioned at the numerical value interval of O/W (oil-in-water type), the emulsion now forming is O/W type, otherwise is w/o type emulsion.Through test of many times, this experiment has drawn the optimum mixture ratio example of Tween 80 with class of department 80, and the chlorine tetramethrin emulsion of formation is O/W type, and the most stable.
2, the present invention is not containing organic solvent, and carrier is all water, can be country and saves a large amount of energy, meets the international trend of low-carbon (LC), energy-saving and environmental protection.Without obvious irritation, to human-body safety, simultaneously because the carrier of preparation is all water, nonflammable to skin, make product all quite safe in storage, transport and use procedure.In compound method, being different from general chloramines chrysanthemum ester oil emulsion adds multiple organic solvent (as ethanol, kerosene etc.) to dissolve material medicine, the 2nd, directly adopt raw material to dissolve raw material (dissolving tetramethrin under permethrin hot conditions), separately add surfactant and water is formulated, simplify technique, provide cost savings, strengthened curative effect.
3, aqueous emulsion part particle diameter of the present invention (1000nm) has reached nanoscale, approaches the rank of nano-emulsion.Because spherolite particle diameter is little and quantity is many, can make medicine there is targeting, delayed the speed of medicine from discharging in microballoon simultaneously, make this aqueous emulsion more general missible oil formulation there is more significantly slow release effect; Evenly, the distribution that this is more conducive to medicine, has strengthened and has killed mosquito effect spherolite size.
4. pH value scope of the present invention is between 5.5～6.5.PH value is a key factor that affects emulsion stability.Because this product main component is water, the PH of other raw materials is all neutrality, so this product P H approaches the pH value of experiment water.Too low pH value makes this aqueous emulsion produce some curdled milk bulks, and proterties changes; PH value is too high, and layering easily occurs solution.Recording best pH value of the present invention by test of many times is 6.0.
5. it is very similar to milk in proterties that the milk flavour adding in the present invention makes it, and milky and tool milk fragrance are distinguished to some extent with general mosquito repellent emulsion proterties, simultaneously is more conducive to lure kill more mosquitos and flies.
The present invention is through stability test, and proterties, content have no significant change, act normally; The standard of recommending according to U.S. FDA, the term of validity of this aqueous emulsion is 2 years.Simultaneously clinical trial shows, chlorine tetramethrin aqueous emulsion of the present invention is to skin without obvious irritation, and its repelling and killing bugs effect is remarkable.The particle disperseing in water after chlorine tetramethrin aqueous emulsion thin up is thinner than missible oil, and permeability strengthens, and absorption ratio improves simultaneously, and repelling and killing bugs successful gets a promotion, and therefore drug effect is more effective than missible oil.This product is applicable to family, public environment, peasant household's cultivation, to sting, sting, harass the mankind throughout the year, the insects such as the mosquitos and flies, lice, flea of harm domestic animal (fowl) growth have well to be killed and repellent action, and to control livestock itch mite, and the manure pit maggot of going out has special efficacy.
In a word, the environmental type preparation that chlorine tetramethrin aqueous emulsion prepared by the present invention is good stability, not containing organic solvent, low production cost, repelling and killing bugs effect is remarkable.Its preparation technology is simple, and steady quality is to person poultry safety, easy to use, reliable for effect, is applicable to family, public place, plant etc., meets the development trend of international environmental protection.
Brief description of the drawings
Fig. 1 is chlorine tetramethrin aqueous emulsion spherolite distribution map (16 × 100 times) under microscope;
Fig. 2 is chlorine tetramethrin aqueous emulsion particle diameter distribution map.
Embodiment
Embodiment 1
The raw material that contains following weight in the chlorine tetramethrin aqueous emulsion of described 1000mL repelling and killing bugs:
Embodiment 2
The raw material that contains following weight in the chlorine tetramethrin aqueous emulsion of described 1000mL repelling and killing bugs:
Embodiment 3
The raw material that contains following weight in the chlorine tetramethrin aqueous emulsion of described 1000mL repelling and killing bugs:
Embodiment 4
The preparation and property of chlorine tetramethrin aqueous emulsion is measured
1 material
1.1 main agents:
Tetramethrin (Shandong, Wuhan Hua Yue reaches Chemical Co., Ltd.); Permethrin (Shandong, Wuhan Hua Yue reaches Chemical Co., Ltd.); Tetramethrin reference substance (Chinese veterinary drug feed is supervised institute); Permethrin reference substance (Chinese veterinary drug feed is supervised institute); Tween 80 (analyze pure, Tianjin great Mao chemical reagent factory); Department class 80 (analyze pure, Tianjin great Mao chemical reagent factory); Milk flavour (Shanghai Yi Kesaiting spices Co., Ltd).
1.2 instrument
HHS type electric-heated thermostatic water bath (Medical Equipment Plant of Shanghai Boxun Industrial Co., Ltd.); PHS-25 type acidometer (Shanghai Precision Scientific Apparatus Co., Ltd); SG2200HE ultrasonic cleaner (Shanghai hat hypersonic sound Instrument Ltd.); Electronic analytical balance AUW120D (Japanese Shimadzu); Beaker (assay apparatus Co., Ltd of Changsha BOCO); Efficient liquid phase chromatographic analysis instrument (Agilent1200, Agilent Technologies of the U.S.); Magnetic stirring apparatus (Mei Ying Pu, Shanghai instrument and meter Manufacturing Co., Ltd); Electron microscope (Japanese Shimadzu).
1.3 experimental animal
Kunming is 30 of healthy mices, body weight 19 ± 2g, and male and female half and half, are purchased from zoopery portion of Hunan College of Traditional Chinese Medicine.
2 methods
2.1 preparation technologies: to prepare total amount as 1000mL chlorine tetramethrin aqueous emulsion is as example.
First, prepare tetramethrin 5g, permethrin 15g, milk flavour 5g, Tween 80 (Tween-80) 50mL, 80 (Span-80) 10mL of class of department, prepare water 900mL.Then preparation as follows:
(1) with 15g permethrin, 5g tetramethrin is dissolved under 90 DEG C of conditions, stir as A liquid;
(2) taking 80 (Span-80) of class of 50mL Tween 80 (Tween-80), 10mL department and mix, is B liquid;
(3) A liquid and B liquid being uniformly mixed under 55 DEG C of conditions, is C liquid;
(4) under stirring, in C liquid, add the purified water of isothermal, solution becomes white emulsion very soon;
(5) the milk flavour solution that adds prior water to dissolve in emulsion, adds water to 1000mL.
2.2 Performance Detection
2.2.1 proterties: by visually observing, its proterties is made to Primary Evaluation.
2.2.2 emulsion spherolite size measurement and distribution: the chloramines chrysanthemum ester solution taking a morsel, add water after 100 times of dilutions, get one after another drop ofly on slide, after covered, under electron microscope high power camera lens, observe emulsion coated spherolite shape, particle diameter and distribution situation.
2.2.3 stability experiment: the chlorine tetramethrin aqueous emulsion of three batches is put at 5～10 DEG C, respectively at 0,4,8,12 month, its proterties, pH value, lamination, content are carried out to Observe and measure.
2.2.4 irritation test
Get 20 of small white mouses, with 8%Na2S solution coating, in the back of small white mouse, preserved skin loses hair or feathers.In depilation district's medication, continuous use 7d, observes medication skin and whether occurs redness or patch.
3 results
3.1 proterties: this product is the fine and smooth shape emulsion of milky, tool milk fragrance.
3.2 emulsion spherolite size measurement and distribution (the results are shown in Figure 1 and Fig. 2)
Can be found out by Fig. 1 and Fig. 2, the microspherulite diameter of the chlorine tetramethrin aqueous emulsion that this experiment is done is less, and individual difference is little, is mainly positioned between 2-4 μ m, and micro-Microscopic observation spherolite is evenly distributed, good fluidity.
3.3 stability test result:
The results are shown in Table 1:
Table 1 reserved sample observing experimental result
It is very little that the proterties of chlorine tetramethrin aqueous emulsion, content are subject to the impact of external environment (resting period and temperature) as can be seen from Table 1, and stability experiment is qualified.
3.4 irritation test
Observed result shows, obvious redness or patch do not appear in mouse agents area, show this preparation to skin without obvious irritation.
Embodiment 5
The test of chlorine tetramethrin aqueous emulsion mosquito repellent
1. materials and methods
1.1 materials: white polyester mosquito net 184cmx90cmx160cm, the female insect that after aedes albopictus emergence, 2～3 ages in days are not sucked blood; Chlorine tetramethrin aqueous emulsion (this laboratory self-control); Chloramines chrysanthemum ester solution spray (Chengdu company).
1.2. method: immerse mosquito-proof dressing liquid (antimosquito finishing agent 130g/L, adhesive 40g/L, bath raio 1:8) after commodity mosquito net is wetting, (100 DEG C, 30S) are dried → baked in 40 DEG C of dipping 30min → dehydration → 60 DEG C.
By each the mosquito net before and after mosquito-proof arrangement 8 tops, be placed in the more discarded room of mosquito, place at the mosquito net arranging and unfinished mosquito net interval, and evening, 18:00～20:30 observes mosquito number and activity situation, adds up mosquito mortality morning next day.Identical test repeats 2 times, guarantees that the data that obtain are reliable.By the mosquito net analog family washing process washing after mosquito-proof arrangement 5 times, then test.Using mosquito populations inside and outside not arranging mosquito net as radix, calculate mosquito repellent rate according to the dead quantity of mosquito inside and outside the mosquito net arranging.
Kill mosquito test: with reference to GB/T17322.10-1998 " the indoor harmacological effect evaluation of agriculture chemical registration hygienic insecticide; Repellant ", first carry out attack test, in grow × wide × high mosquito cage for 40cmx30cmx30cm, put into approximately 100 aedes albopictus, expose 4cmx4cm skin at the back of the hand, remainder tightly covers.Hand is stretched into 2min in mosquito cage, and the examination worm that comes to stop falling for attack is qualified, can be used for repellency test more than 30 persons.Select examination worm and 1 volunteer that attack is qualified, at people's the each 4cmx4cm skin exposing wherein of both hands back, tightly cover remainder.The mosquito netting for preventing mosquito cloth that the expose portion of a hand was processed with the chlorine tetramethrin aqueous emulsion cutting covers, and the expose portion of another hand covers with the mosquito netting for preventing mosquito cloth that chloramines chrysanthemum ester solution spray was processed, and as a control group, separately establishes blank group.Hand is stretched into 2min in the cage that is placed with the qualified mosquito of attack, observe the invasion and attack situation of mosquito, all above persons of 5s that stops to fall on fabric are designated as invasion and attack once.Mosquito net after mosquito-proof arrangement is placed respectively after 1 week, 2 weeks, 3 weeks, 4 weeks and repeated above-mentioned test.
Knock down and lethal test: with reference to GB13917.8-1992 (the indoor harmacological effect evaluation of agriculture chemical registration hygienic insecticide; Simulated field efficacy testing method ", test period section is 19:00～22:00, indoor central authorities at area 15 ㎡, height 2.8m hang up the mosquito net through mosquito-proof arrangement, and in mosquito net, put into mosquito luring lamp and mosquito-attracting reagent simultaneously, fasten door and window, discharge 100 examination worms, every 30min records the examination borer population of once knocking down, then collect and be transferred in clean dependent insect cage all trying worm, and with 5% syrup cotton balls feed, when 24h, check dead examination borer population, with blank test, rate of knockdown and lethality are proofreaied and correct.Mosquito net after mosquito-proof arrangement is placed respectively after 1 week, 2 weeks, 3 weeks, 4 weeks and repeated above-mentioned test.
2. the finishing effect of mosquito netting for preventing mosquito
2.1 repelling effects (concrete effect is in table 2).
The repelling effect of table 2 mosquito netting for preventing mosquito
Note: 1
#～5
#for volunteer's numbering, A is mosquito-proof group of chlorine tetramethrin aqueous emulsion, and B is the mosquito-proof control group of chloramines chrysanthemum ester solution spray, and C is blank group.
As can be seen from Table 2, on A, B group mosquito netting for preventing mosquito cloth, the invasion and attack number of times of mosquito is obviously less than blank group.Illustrate through the mosquito net of mosquito-proof arrangement and there is obvious mosquito-proof effect; We are not difficult to find out that A group mosquito invasion and attack number of times is obviously less than B group simultaneously.Along with the prolongation of standing time, on mosquito netting for preventing mosquito cloth, the invasion and attack total degree of mosquito increases gradually, and A group mosquito recruitment is still less than B group, illustrates that this chlorine tetramethrin aqueous emulsion has good sustained release performance, has ensured the persistence of mosquito-proof effect.
2.2 kill mosquito effect (concrete outcome is in table 3).
Table 3 mosquito netting for preventing mosquito kill mosquito effect
Note: A is mosquito-proof group of chlorine tetramethrin aqueous emulsion, and B is the mosquito-proof control group of chloramines chrysanthemum ester solution spray.
As can be seen from Table 3, along with the prolongation of observation time, mosquito rate of knockdown increases gradually, shows that the mosquito net after mosquito-proof arrangement has good down effect; For the mosquito netting for preventing mosquito of different standing times, A group mosquito rate of knockdown and lethality are apparently higher than B group; Along with placing the increase of all numbers, two groups of mosquito netting for preventing mosquito rate of knockdown and lethality to mosquito all declines to some extent, but the fall of A group is starkly lower than B group, has embodied chlorine tetramethrin aqueous emulsion and has had and kill the superiority that mosquito effect is strong and lasting with respect to chloramines chrysanthemum ester solution spray.
3. conclusion
Chlorine tetramethrin aqueous emulsion repelling and killing bugs successful prepared by this laboratory, and there is good durability, to person poultry safety, desinsection wide spectrum, easy to use, economical and practical, be convenient to promote.
Claims (5)
1. for a chlorine tetramethrin aqueous emulsion for repelling and killing bugs, it is characterized in that, aqueous emulsion is made up of the raw material of following weight described in 1000mL:
2. chlorine tetramethrin aqueous emulsion as claimed in claim 1, is characterized in that, aqueous emulsion is made up of the raw material of following weight described in 1000mL:
3. the preparation method of chlorine tetramethrin aqueous emulsion as claimed in claim 1 or 2, in 1000mL aqueous emulsion, described method comprises the steps:
(1) take tetramethrin and permethrin by the weight described in claim 1 or 2, under 80 DEG C～100 DEG C conditions, dissolve tetramethrin with permethrin, obtain A liquid;
(2) take Tween 80 and Si Ban 80 by the weight described in claim 1 or 2, mix, obtain B liquid;
(3) A liquid and B liquid are uniformly mixed under 40～60 DEG C of conditions, obtain C liquid;
(4) to the water that adds 40～60 DEG C in C liquid, obtain white emulsion, then add water to 1000mL, obtain chlorine tetramethrin aqueous emulsion.
4. method as claimed in claim 3, is characterized in that, described step (1) is dissolved tetramethrin with permethrin under 90 DEG C of conditions.
5. method as claimed in claim 4, is characterized in that, step (3) is under 55 DEG C of conditions, to mix A liquid and B liquid.
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| CN110638675A (en) * | 2019-09-17 | 2020-01-03 | 江西农业大学 | Terpenoid repellent R2 microemulsion and preparation method thereof |
| CN111096328A (en) * | 2019-10-10 | 2020-05-05 | 江苏生久农化有限公司 | Insecticidal aqueous emulsion without solvent and preparation method thereof |
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