CN104068062B - Chlorine tetramethrin aqueous emulsion of a kind of repelling and killing bugs and preparation method thereof - Google Patents
Chlorine tetramethrin aqueous emulsion of a kind of repelling and killing bugs and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of chlorine tetramethrin aqueous emulsion (O/W) for repelling and killing bugs and preparation method thereof, described 1000mL aqueous emulsion is made up of the raw material of following weight: tetramethrin: 3 ~ 7g; Permethrin: 13 ~ 17g; Tween 80 (Tween-80): 48 ~ 52mL; Department class 80 (Span-80): 18 ~ 22mL; Milk flavour: 3 ~ 7g.Chlorine tetramethrin aqueous emulsion prepared by the present invention is environmental type preparation, not containing organic solvent, and low production cost, repelling and killing bugs Be very effective.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.
Description
Technical field
The invention belongs to technical field of medicine, chlorine tetramethrin aqueous emulsion being specifically related to a kind of repelling and killing bugs and preparation method thereof.
Background technology
The repelling and killing bugs medicine that current China market is sold is still based on missible oil formulation, because missible oil excitant is large, solvent is inflammable and contaminated environment, simultaneously because new drug development needs to drop into substantial contribution, under current economic form, emphasis is turned to the exploitation of novel form by many companies.Aqueous emulsion (Emulsioninwater, EW) being take water as the class emulsion dosage form (being O/W type) of dispersion medium, particle diameter is between 0.1 ~ 50.0 μm, outward appearance is milky, continuous phase is water, in formula, consumption of organic solvent is less or not containing organic solvent, compared with traditional veterinary dosage form---and missible oil has the advantages such as little, the nonflammable and use safety of 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, chlorine tetramethrin aqueous emulsion providing a kind of repelling and killing bugs and preparation method thereof, 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, it is characterized in that, aqueous emulsion described in 1000mL is made up of the raw material of following weight:
Preferably, 3 ~ 7g can also be contained in aqueous emulsion described in 1000mL, preferred 5g milk flavour.
Preferably, form containing, for example the raw material of lower 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 any one of claims 1 to 3, 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 any one of claims 1 to 3, mix, obtain B liquid;
(3) A liquid and B liquid are uniformly mixed under 40 ~ 60 DEG C of conditions, obtain C liquid;
(4) in C liquid, add the water of 40 ~ 60 DEG C, obtain white emulsion, then add water to 1000mL, obtain chlorine tetramethrin aqueous emulsion.
Preferably, milk flavour solution can also be added in step (4) gained white emulsion, then add water to 1000mL.
Preferably, described step (1) dissolves tetramethrin with permethrin under 90 DEG C of conditions;
Preferably, step (3) is under 55 DEG C of conditions, mix A liquid and B liquid.
Tetramethrin, permethrin, Tween 80 (Tween-80), class 80 of department (Span-80), milk flavour etc. are obtained finished product through proper proportion dissolving, mixing, stirring, packing by the present invention, are applied to repelling and killing bugs.Its innovation is:
1, surface active agent tween 80 mixes with class 80 of department to be applied in chlorine tetramethrin aqueous emulsion by the present invention first, and the best configuration proportion both drawing in this aqueous emulsion is 5:1.The stability of emulsion is the topic that in emulsion, is quite disputed on always; preparing the most incidental problem of emulsion is exactly oil breast separation and layering; and the improper use of surfactant i.e. layering soon after emulsion often can be made to be formed or to be formed, so the selection of surfactant and compatibility thereof are the key technologies of this test.Tween 80, class 80 of department are all nonionic surface active agent and emulsifier, Tween 80 is O/W type emulsifier, nontoxic non-stimulated, difficult combustion, water-soluble, have excellent emulsification and soak, disperse and permeance property, class 80 of department is W/O (Water-In-Oil) type emulsifier, for non-aqueous emulsifier, these two kinds of emulsifier all have clinically to be applied more widely.Through By consulting literatures and clinical testing, confirm these two kinds of surfactants in proportion effect used in combination be better than single surfactant, and the two mixed proportion and its hydrophilic lipophilic balance (HLB value) are closely related, when the two mixed proportion makes HLB value be positioned at the numerical intervals of O/W (oil-in-water type), the emulsion now formed is O/W type, otherwise is w/o type emulsion.Through test of many times, this experiment has shown that Tween 80 is routine with the optimum mixture ratio of class 80 of department, 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, meet the international trend of low-carbon (LC), energy-saving and environmental protection.To skin without obvious irritation, to human-body safety, simultaneously because the carrier of preparation is all water, nonflammable, make product all quite safe in storage, transport and use procedure.Compound method is different from general chloramines chrysanthemum ester oil emulsion and adds multiple organic solvent (as ethanol, kerosene etc.) dissolving material medicine, two is 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, enhance curative effect.
3, aqueous emulsion part particle diameter (1000nm) of the present invention reaches nanoscale, close to the rank of nano-emulsion.Because spherolite particle diameter is little and quantity is many, medicine can be made to have targeting, delayed the speed that medicine discharges in microballoon simultaneously, make the more general missible oil formulation of this aqueous emulsion have more significantly slow release effect; Spherolite size is even, and this is more conducive to the distribution of medicine, enhances and kills mosquito effect.
4. pH value range of the present invention is between 5.5 ~ 6.5.PH value is the key factor affecting emulsion stability.Because this product main component is water, the PH of other raw materials is all neutrality, so this product P H is close to the pH value of experiment water.It is block that too low pH value makes this aqueous emulsion produce some curdled milks, and proterties changes; PH value is too high, then solution easily layering occurs.Recording best pH value of the present invention by test of many times is 6.0.
5. the milk flavour added in the present invention makes it very similar to milk in proterties, milky and tool milk fragrance, distinguishes to some extent with general mosquito repellent emulsion proterties, is more conducive to luring simultaneously and kills more mosquitos and flies.
The present invention is through stability test, and proterties, content have no significant change, act normally; According to the standard that U.S. FDA is recommended, the term of validity of this aqueous emulsion is 2 years.Simultaneously clinical trial shows, chlorine tetramethrin aqueous emulsion of the present invention to skin without obvious irritation, its repelling and killing bugs Be very effective.The particle disperseed in water after chlorine tetramethrin aqueous emulsion thin up is thinner than missible oil, and permeability strengthens, and simultaneously stability rate improves, 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 stining, sting, harass the mankind throughout the year, harm domestic animal (fowl) insect such as mosquitos and flies, lice, flea that grows has well to be killed and repellent action, and to control livestock itch mite, and manure pit maggot of going out has special efficacy.
In a word, chlorine tetramethrin aqueous emulsion prepared by the present invention is the environmental type preparation of good stability, not containing organic solvent, and low production cost, repelling and killing bugs Be very effective.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.
Accompanying drawing explanation
Fig. 1 is chlorine tetramethrin aqueous emulsion spherolite distribution map (16 × 100 times) under microscope;
Fig. 2 is chlorine tetramethrin aqueous emulsion grain size distribution.
Embodiment
Embodiment 1
Containing, for example the raw material of lower weight in the chlorine tetramethrin aqueous emulsion of described 1000mL repelling and killing bugs:
Embodiment 2
Containing, for example the raw material of lower weight in the chlorine tetramethrin aqueous emulsion of described 1000mL repelling and killing bugs:
Embodiment 3
Containing, for example the raw material of lower 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 measures
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 supervision institute); Permethrin reference substance (Chinese veterinary drug feed supervision institute); Tween 80 (analyzing pure, Tianjin great Mao chemical reagent factory); Class 80 of department (analyzing 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 system healthy mice 30, body weight 19 ± 2g, male and female half and half, are purchased from Hunan College of Traditional Chinese Medicine's Animal Experimental.
2 methods
2.1 preparation technologies: to prepare total amount for 1000mL chlorine tetramethrin aqueous emulsion.
First, prepare tetramethrin 5g, permethrin 15g, milk flavour 5g, Tween 80 (Tween-80) 50mL, department class 80 (Span-80) 10mL, prepare water 900mL.Then prepare as follows:
(1) with 15g permethrin, 5g tetramethrin is dissolved under 90 DEG C of conditions, be stirred for A liquid;
(2) taking 50mL Tween 80 (Tween-80), class of 10mL department 80 (Span-80) mixes, is B liquid;
(3) A liquid and B liquid being uniformly mixed under 55 DEG C of conditions, is C liquid;
(4) under stirring, add the purified water of isothermal in C liquid, solution becomes white " milky " liquid very soon;
(5) in emulsion, add milk flavour solution good by water-soluble solution in advance, add water to 1000mL.
2.2 Performance Detection
2.2.1 proterties: by visually observing, makes Primary Evaluation to its proterties.
2.2.2 emulsion spherolite size measurement and distribution: the chloramines chrysanthemum ester solution taken a morsel, adds water 100 times after diluting, and gets one after another drop of on slide, observes the spherolite shape of emulsion bag quilt, size and distribution situation after covered under electron microscope high power camera lens.
2.2.3 stability experiment: at the chlorine tetramethrin aqueous emulsion of three batches is put 5 ~ 10 DEG C, respectively at 0,4,8,12 month, Observe and measure is carried out to its proterties, pH value, lamination, content.
2.2.4 irritation test
Get small white mouse 20, with the back of 8%Na2S solution coating in small white mouse, depilation preserved skin.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, and be mainly positioned between 2-4 μm, basis of 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
The proterties of chlorine tetramethrin aqueous emulsion, content are very little by 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, obviously red and swollen or patch does not appear in mouse agents area, shows this preparation to skin without obvious irritation.
Embodiment 5
Chlorine tetramethrin aqueous emulsion mosquito repellent is tested
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 (self-control of this laboratory); 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, 40 DEG C of dipping 30min → dehydration → 60 DEG C are dried → are baked (100 DEG C, 30S).
By each for the mosquito net before and after mosquito-proof arrangement 8 tops, be placed in the more discarded room of mosquito, the mosquito net arranged and the placement of unfinished mosquito net interval, in 18:00 ~ 20:30 observation in evening mosquito number and activity situation, morning next day adds up mosquito mortality.Identical test repeats 2 times, guarantees that the data obtained are reliable.Mosquito net analog family washing process after mosquito-proof arrangement is washed 5 times, then tests.As radix, mosquito repellent rate is calculated according to mosquito death toll gauge inside and outside the mosquito net arranged not arrange mosquito populations inside and outside mosquito net.
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, growing × and wide × high for putting into about 100 aedes albopictus in the mosquito cage of 40cmx30cmx30cm, expose 4cmx4cm skin at the back of the hand, remainder tightly covers.Hand is stretched into 2min in mosquito cage, the examination worm coming to stop to fall is qualified for attack more than 30 persons, can be used for repellency test.The examination worm selecting attack qualified and 1 volunteer, respectively expose 4cmx4cm skin wherein at the both hands back of people, tightly cover remainder.The expose portion of a hand covers with the mosquito netting for preventing mosquito cloth of the chlorine tetramethrin aqueous emulsion process cut, and the mosquito netting for preventing mosquito cloth of the expose portion chloramines chrysanthemum ester solution spray process of another hand covers, and as a control group, separately establishes blank group.Hand is stretched into 2min in the cage being placed with the qualified mosquito of attack, observes the invasion and attack situation of mosquito, all more than 5s persons that stops to fall on fabric are designated as invasion and attack once.Above-mentioned test is repeated after mosquito net after mosquito-proof arrangement is placed 1 week, 2 weeks, 3 weeks, 4 weeks respectively.
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, the mosquito net through mosquito-proof arrangement is hung up in the indoor central authorities of area 15 ㎡, height 2.8m, and put into mosquito luring lamp and mosquito-attracting reagent in mosquito net simultaneously, fasten door and window, discharge 100 examination worms, every 30min records the examination borer population once knocked down, then collect all trying worm and be transferred in clean dependent insect cage, and feed with 5% syrup cotton balls, check during 24h and extremely try borer population, with blank test, rate of knockdown and lethality are corrected.Above-mentioned test is repeated after mosquito net after mosquito-proof arrangement is placed 1 week, 2 weeks, 3 weeks, 4 weeks respectively.
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 that the mosquito net through mosquito-proof arrangement has 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, ensure that 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 time, A group mosquito rate of knockdown and lethality are apparently higher than B group; Along with the increase of placing all numbers, two groups of mosquito netting for preventing mosquito decline all to some extent to the rate of knockdown of mosquito and lethality, but the fall of A group is starkly lower than B group, embodies chlorine tetramethrin aqueous emulsion and have relative to chloramines chrysanthemum ester solution spray and kill the strong and lasting superiority of mosquito effect.
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 described in 1000mL is made up of the raw material of following weight:
2. chlorine tetramethrin aqueous emulsion as claimed in claim 1, it is characterized in that, aqueous emulsion described in 1000mL is made up of the raw material of following weight:
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) in C liquid, add the water of 40 ~ 60 DEG C, obtain white emulsion, then add water to 1000mL, obtain chlorine tetramethrin aqueous emulsion.
4. method as claimed in claim 3, it is characterized in that, described step (1) dissolves tetramethrin with permethrin under 90 DEG C of conditions.
5. method as claimed in claim 4, it is characterized in that, step (3) is under 55 DEG C of conditions, mix A liquid and B liquid.
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