1%米尔贝霉素微乳剂的研制
摘要
近年来,发达国家对农药制剂中使用有机溶剂的限制日益严格,从而促使农药剂型要不断更新和发展,其中水性化制剂就是农药剂型发展的主导方向之一。因此,以水部分或全部代替乳油中有机溶剂的微乳剂和水乳剂便应运而生,使其成为农药新剂型而得到开发应用。米尔贝霉素是一种高效杀虫剂,是十六元大环内酯混合物,对各种螨类,蚜虫效果较好,对生长在蔬菜、棉花、小麦、水稻、苹果等的多种害虫也有较好的防治效果,杀虫谱较广,目前在我国农业生产中还没有相应的杀虫剂产品。本研究研制开发了1%米尔贝霉素微乳剂,并对其进行了系统的配方试验。明确了其对菜豆红蜘蛛、菜蚜杀虫效果,并进行了示范和推广应用。
本项研究利用化学和生物方法,系统研究米尔贝霉素理化特性,表面活性剂对米尔贝霉素的作用;明确1%米尔贝霉素微乳剂加工工艺,研制开发了1%米尔贝霉素微乳剂,并对其进行系统试验,对菜豆红蜘蛛、蚕豆蚜虫作用效果进行了生物验证试验。试验的研究结果如下:
1.对国内未报道过的1%米尔贝霉素微乳剂的配方进行了筛选,根据其理化性质和原料成本,优选出乙酸乙酯为溶剂和水为介质,用蓖麻油聚氧乙烯醚EL-90和农乳500,按8:2的比例混用,形成复合表面活性剂,用异丙醇为助表面活性剂。采用与乳油相似的加工工艺即可加工出1%米尔贝霉素微乳剂。其中米尔贝霉素含量为2.5%,乙酸乙酯为8%,EL-90为12.8%、农乳500为3.2%、异丙醇为2%,乙二醇5%、光稳定剂1010为1%,丙三醇为3%,水补齐至100%。
2.本文采用高效液相色谱法,以甲醇+水为流动相,测定1%米尔贝霉素微乳剂中米尔贝霉素有效成分的含量。其标准偏差为0.0030、变异系数为0.2920%、平均回收率分别为99.8%,线性相关系数为0.9989。根据试验结果符合相应的国家标准,制定出了企业的产品质量标准。
3.按FAO标准对1%米尔贝霉素微乳剂进行了贮存稳定性试验,常温贮存3个月、6个月、12个月的分解率分别为1.07%、1.43%、1.87%;低温稳定性(-5±0.1℃,14天),在轻度振动后,无可见分离颗粒和油状物,平均分解率为2.37%;热贮稳定性(-54±2℃,14天),相对的分解率平均为1.93%。米尔贝霉素含量≥1.03%,1%米尔贝霉素微乳剂每毫升质量为1.0623g,pH值为5.0~6.0,透明温度区域为-9.6～73.4℃,1min之内持久起泡量≤25 ml。
4.本文使用高效液相色谱进行线性分析,同时进行了回收率和分析方法精密度测定。经试验回收率为99.80%;分析方法标准差为0.0030;变异系数为0.2920%。
5.在对1%米尔贝霉素微乳剂配方确定之后,进行了对新开发农药的室内毒力和盆栽防效测定。通过室内毒力试验,得出1%米尔贝霉素微乳剂对菜豆红蜘蛛和菜蚜的LC50,分别为0.0823mg?L-1和0.2022mg?L-1。
In recent years, the limit to the organic solvent for the agricultural chemicals preparation in the developed country has been more stricted. thus urged the agricultural chemicals dosage-form to renew unceasingly and develop, the water-character preparation was one of agricultural chemicals dosage-form development leading directions. Therefore, the micro emulsion and the aqueous emulsion that all or partial part the organic solvent replace by water arises at the historic moment, and it become the agricultural chemicals new dosage-form to obtain the development application.
Milbemiycins is one kind of highly effective pesticide, is 16-membered ring macrolides mixtures. It is efficient on acarine and ophid. and to the vegetables, the cotton, the wheat, the paddy rice, the apple on and many kinds of harmful insects also has the good control efficiency. The insect disinfestation spectrum is broad, and there is no reporting of corresponding pesticide product in our country agricultural production. This research has developed 1% milbemycins micro emulsion, and has carried on system's formula experiment to it. Has been clear about it to the kidney bean red spider, the cabbage aphid insect disinfestation effect, and has carried on the demonstration and the promoted application.
In this study, the physics and chemistry characteristic of Milbemycins have been researched systematically with chemistry and the biological method. And the surface active agent function to the Milbemycins has also been researched. Identify the product quality of 1% Milbemycins micro emulsion. The 1% Milbemycins micro emulsion has been developed successfully.The pharmacodynamic test on bean aphid and red mite demonstrate that 1% Milbemycins microemulsion were effective with both of the two field-pests.
The results as following:
1. In this paper, the composition and preparation of 1% Milbemycins microemulsion were introduced, which have not been reported in our country. After a serious of selection experiments of different solvent, surfactants, co-solvents, antifreeze , antiblowing, light stabilizer and water, the results showed that the optimum formulation are as follows Milbemycins 2.5%, acetidin 8%, surfactants 16% (EL-90 12.8%, pesticide emulsifier 3.2%), isopropyl alcohol 2%, ethylene glycol 5%, light stabilize1% and water. The physico-chemical property was detected. The results showed that all physico-chemical properties of Milbemycins microemulsion were well tally with the national standards.
2. RP-HPLC is conducted in this study. Methanol and water are selected as mobile phase, the containing of the micellar emulsion of 1% Milbemycins microemulsion is determined. The result as following: standard deviation is 0.0030, coefficient of variability is 0.2920%, recovery rate is 99.8%, correlation coefficient is 0.9989. Its standard deviation, coefficient of variability and average recovery rate are colinearity coefficient correlation.
3. The micro emulsion carried on the storing stability test according to the FAO standard to 1% Milbemycins, the normal temperature has stored 3 months, 6 months, 12 month-long rates of dissociation respectively is 1.07%, 1.43%, 1.87%; Low temperature stability (-5±0.1℃,14day), after mild vibration, does not have separates the pellet and greasy obviously, the average rate of dissociation is 2.37%; The heat stores the stability (-54±2℃,14day), the relative rate of dissociation is 1.93% equally. Mil Bei Meisu the content≥1.03%, 1% mil Bei Meisu micro emulsion each milliliter quality is the 1.0623g/ml, pH value is 5.0~6.0, transparent temperature province for - 9.6~73.4℃,1min within lasting bubbling quantity≤25 ml.
4. This research uses the HPLC(high performance liquid chromatogram) to carry on the linearity analysis, the returns-ratio and the analysis method accuracy determination. After the experiment indicate: the recovery rate is 99.80%; the analysis method standard deviation is 0.0030; the coefficient of variation is 0.2920%.
5. After the formula determination of 1% Milbemycins micellar emulsion, has carried on to the new development pesticide indoor toxicity and the bonsai against effect determination. Through the indoor toxicity test, obtains 1% Milbemycins micro emulsion to the kidney bean red spider and cabbage aphid's LC50, respectively is 0.0823mg?L-1 and 0.2022mg?L-1.
本项研究利用化学和生物方法,系统研究米尔贝霉素理化特性,表面活性剂对米尔贝霉素的作用;明确1%米尔贝霉素微乳剂加工工艺,研制开发了1%米尔贝霉素微乳剂,并对其进行系统试验,对菜豆红蜘蛛、蚕豆蚜虫作用效果进行了生物验证试验。试验的研究结果如下:
1.对国内未报道过的1%米尔贝霉素微乳剂的配方进行了筛选,根据其理化性质和原料成本,优选出乙酸乙酯为溶剂和水为介质,用蓖麻油聚氧乙烯醚EL-90和农乳500,按8:2的比例混用,形成复合表面活性剂,用异丙醇为助表面活性剂。采用与乳油相似的加工工艺即可加工出1%米尔贝霉素微乳剂。其中米尔贝霉素含量为2.5%,乙酸乙酯为8%,EL-90为12.8%、农乳500为3.2%、异丙醇为2%,乙二醇5%、光稳定剂1010为1%,丙三醇为3%,水补齐至100%。
2.本文采用高效液相色谱法,以甲醇+水为流动相,测定1%米尔贝霉素微乳剂中米尔贝霉素有效成分的含量。其标准偏差为0.0030、变异系数为0.2920%、平均回收率分别为99.8%,线性相关系数为0.9989。根据试验结果符合相应的国家标准,制定出了企业的产品质量标准。
3.按FAO标准对1%米尔贝霉素微乳剂进行了贮存稳定性试验,常温贮存3个月、6个月、12个月的分解率分别为1.07%、1.43%、1.87%;低温稳定性(-5±0.1℃,14天),在轻度振动后,无可见分离颗粒和油状物,平均分解率为2.37%;热贮稳定性(-54±2℃,14天),相对的分解率平均为1.93%。米尔贝霉素含量≥1.03%,1%米尔贝霉素微乳剂每毫升质量为1.0623g,pH值为5.0~6.0,透明温度区域为-9.6～73.4℃,1min之内持久起泡量≤25 ml。
4.本文使用高效液相色谱进行线性分析,同时进行了回收率和分析方法精密度测定。经试验回收率为99.80%;分析方法标准差为0.0030;变异系数为0.2920%。
5.在对1%米尔贝霉素微乳剂配方确定之后,进行了对新开发农药的室内毒力和盆栽防效测定。通过室内毒力试验,得出1%米尔贝霉素微乳剂对菜豆红蜘蛛和菜蚜的LC50,分别为0.0823mg?L-1和0.2022mg?L-1。
In recent years, the limit to the organic solvent for the agricultural chemicals preparation in the developed country has been more stricted. thus urged the agricultural chemicals dosage-form to renew unceasingly and develop, the water-character preparation was one of agricultural chemicals dosage-form development leading directions. Therefore, the micro emulsion and the aqueous emulsion that all or partial part the organic solvent replace by water arises at the historic moment, and it become the agricultural chemicals new dosage-form to obtain the development application.
Milbemiycins is one kind of highly effective pesticide, is 16-membered ring macrolides mixtures. It is efficient on acarine and ophid. and to the vegetables, the cotton, the wheat, the paddy rice, the apple on and many kinds of harmful insects also has the good control efficiency. The insect disinfestation spectrum is broad, and there is no reporting of corresponding pesticide product in our country agricultural production. This research has developed 1% milbemycins micro emulsion, and has carried on system's formula experiment to it. Has been clear about it to the kidney bean red spider, the cabbage aphid insect disinfestation effect, and has carried on the demonstration and the promoted application.
In this study, the physics and chemistry characteristic of Milbemycins have been researched systematically with chemistry and the biological method. And the surface active agent function to the Milbemycins has also been researched. Identify the product quality of 1% Milbemycins micro emulsion. The 1% Milbemycins micro emulsion has been developed successfully.The pharmacodynamic test on bean aphid and red mite demonstrate that 1% Milbemycins microemulsion were effective with both of the two field-pests.
The results as following:
1. In this paper, the composition and preparation of 1% Milbemycins microemulsion were introduced, which have not been reported in our country. After a serious of selection experiments of different solvent, surfactants, co-solvents, antifreeze , antiblowing, light stabilizer and water, the results showed that the optimum formulation are as follows Milbemycins 2.5%, acetidin 8%, surfactants 16% (EL-90 12.8%, pesticide emulsifier 3.2%), isopropyl alcohol 2%, ethylene glycol 5%, light stabilize1% and water. The physico-chemical property was detected. The results showed that all physico-chemical properties of Milbemycins microemulsion were well tally with the national standards.
2. RP-HPLC is conducted in this study. Methanol and water are selected as mobile phase, the containing of the micellar emulsion of 1% Milbemycins microemulsion is determined. The result as following: standard deviation is 0.0030, coefficient of variability is 0.2920%, recovery rate is 99.8%, correlation coefficient is 0.9989. Its standard deviation, coefficient of variability and average recovery rate are colinearity coefficient correlation.
3. The micro emulsion carried on the storing stability test according to the FAO standard to 1% Milbemycins, the normal temperature has stored 3 months, 6 months, 12 month-long rates of dissociation respectively is 1.07%, 1.43%, 1.87%; Low temperature stability (-5±0.1℃,14day), after mild vibration, does not have separates the pellet and greasy obviously, the average rate of dissociation is 2.37%; The heat stores the stability (-54±2℃,14day), the relative rate of dissociation is 1.93% equally. Mil Bei Meisu the content≥1.03%, 1% mil Bei Meisu micro emulsion each milliliter quality is the 1.0623g/ml, pH value is 5.0~6.0, transparent temperature province for - 9.6~73.4℃,1min within lasting bubbling quantity≤25 ml.
4. This research uses the HPLC(high performance liquid chromatogram) to carry on the linearity analysis, the returns-ratio and the analysis method accuracy determination. After the experiment indicate: the recovery rate is 99.80%; the analysis method standard deviation is 0.0030; the coefficient of variation is 0.2920%.
5. After the formula determination of 1% Milbemycins micellar emulsion, has carried on to the new development pesticide indoor toxicity and the bonsai against effect determination. Through the indoor toxicity test, obtains 1% Milbemycins micro emulsion to the kidney bean red spider and cabbage aphid's LC50, respectively is 0.0823mg?L-1 and 0.2022mg?L-1.
引文
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