CN106106491A - 一种吡唑醚菌酯和咪鲜胺复配水乳剂及其制备方法 - Google Patents
一种吡唑醚菌酯和咪鲜胺复配水乳剂及其制备方法 Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
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Abstract
一种吡唑醚菌酯和咪鲜胺复配水乳剂及其制备方法，涉及柑橘树炭疽病防治技术领域。至少由10份吡唑醚菌酯、30份咪鲜胺、2份安全剂、15份二甲苯、10份烷基酚脂肪醇甲醛树脂聚氧乙烯醚、0.5份盐酸、4.5份乙二醇、1份羧甲基淀粉钠、0.1份二甲基硅油以及补足至100份的水制成。先将盐酸、乙二醇、羧甲基淀粉钠溶解于水中，形成水相；将吡唑醚菌酯和咪鲜胺溶解于二甲苯中，并加入烷基酚脂肪醇甲醛树脂聚氧乙烯醚、二甲基硅油和安全剂形成油相；将油相和水相在乳化釜中混合。本发明以1：3配比混用所复配的40％水乳剂，对柑橘树炭疽病防治可起到明显增效作用范围，而其它配比混用的制剂，均无法达到明显增效作用范围。
Description
技术领域
本发明涉及柑橘树炭疽病防治技术领域，具体是涉及一种吡唑醚菌酯和咪鲜胺复配水乳剂及其制备方法。
背景技术
目前，现有的用于柑橘树炭疽病防治的杀菌组合物，例如中国专利“CN 1582659A”公开了一种“的防治农作物霜霉病、炭疽病的杀菌剂农药和应用”，采用咪鲜胺或其盐类和霜脲氰为主要药效组分制成,咪鲜胺或咪鲜胺盐占农药重量的1～90％，所述的霜脲氰占农药重量的1～90％，所述的赋形剂为余量，三者的重量百分比之和为100％。另有中国专利“CN103004823A”公开了一种“含有吡唑醚菌酯和溴菌腈的复配杀菌组合物”，其有效成分组成为吡唑醚菌酯和溴菌腈，所述吡唑醚菌酯和溴菌腈的重量比为1∶79～79∶1。
发明人经过长期试验验证，该上述几种杀菌组合物主要存在如下缺陷：
1)、通过对上述几种杀菌组合物公开的几种具体配比进行试验，发现对柑橘树炭疽病无法起到良好的防治效果。
2)、针对上述几种杀菌组合物所公开的几种剂型，经过试验验证发现均存在不同问题的缺陷。例如，制成的可湿性粉剂容易引起产品粘结，不易在水中分散悬浮，或堵塞喷头，在喷雾器中道理沉淀等现象，造成喷洒不匀，易使作物局部产生药害，其主要原因在于助剂和填料的选择均存在不同的缺陷。
3)、复配问题，通过对上述几种杀菌组合物公开的几种具体配比进行毒力试验、热贮稳定性试验以及共毒系数测定发现，均无法达到明显的增效作用。
发明内容
本发明的目的之一在于提供一种吡唑醚菌酯和咪鲜胺复配水乳剂，该水乳剂设计合理，对柑橘树炭疽病的防治效果佳，且可实现吡唑醚菌酯和咪鲜胺的明显增效作用。
为实现上述目的，本发明采用了以下技术方案：
一种吡唑醚菌酯和咪鲜胺复配水乳剂，至少由以下重量份的组分制成：
吡唑醚菌酯为线粒体呼吸抑制剂.即通过在细胞色素合成中阻止电子转移。具有保护、治疗、叶片渗透传导作用。吡唑醚菌酯乳油经田间药效试验结果表明对黄瓜白粉病、霜霉病和香蕉黑星病、叶斑病、菌核病等有较好的防治效果。
咪鲜胺为高效、广谱、低毒型杀菌剂，具有预防保护治疗等多重作用，内含咪鲜胺为咪唑类广谱杀菌剂。通过抑制甾醇的生物合成而起作用，无内吸作用，对于子囊菌和半知菌引起的多种病害防效极佳。采用基因诱导技术，激活植物抗病基因表达，速效性好，持效期长，无内吸作用。
本发明的吡唑醚菌酯和咪鲜胺复配水乳剂，其有益效果表现在：
1)、本发明制备的水乳剂在悬浮率、湿筛试验等以及热贮稳定性等方面均明显优于其他配比所制备的产品。
2)、通过实验验证，吡唑醚菌酯和咪鲜胺以1：3配比混用所复配的40％时的吡唑醚菌酯和咪鲜胺复配水乳剂，可起到明显增效作用范围，而其它配比混用的制剂，均无法达到明显增效作用范围。同时，不同配比的实际毒性并未随着理论毒性的增强而提升，实际毒性和理论毒性之间并无有规律性的变化。
本发明的另一目的在于提供一种吡唑醚菌酯和咪鲜胺复配水乳剂的制备方法，先将盐酸、乙二醇、羧甲基淀粉钠溶解于水中，形成水相；将吡唑醚菌酯和咪鲜胺溶解于二甲苯中，并加入烷基酚脂肪醇甲醛树脂聚氧乙烯醚、二甲基硅油和安全剂形成油相；将油相和水相在乳化釜中混合，即得吡唑醚菌酯和咪鲜胺复配水乳剂。
本发明的吡唑醚菌酯和咪鲜胺复配水乳剂的制备方法，制备工艺较为简便，易于工业化生产。
具体实施方式
以下将结合实施例，对本发明进行较为详细的说明。但是，实施例内容仅是对本发明所作的举例和说明，所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，只要不偏离发明的构思或者超越本权利要求书所定义的范围，均应属于本发明的保护范围。
一、吡唑醚菌酯和咪鲜胺复配水乳剂的制备，以及各实施例所制备的水乳剂的各项技术指标的检测结果、热贮稳定性试验结果。
实施例1
40％吡唑醚菌酯和咪鲜胺复配水乳剂，各组分及其重量份如下：
| 成分 | 重量份 |
| 吡唑醚菌酯 | 10 |
| 咪鲜胺 | 30 |
| 安全剂 | 2 |
| 二甲苯 | 15 |
| 烷基酚脂肪醇甲醛树脂聚氧乙烯醚 | 10 |
| 盐酸 | 0.5 |
| 乙二醇 | 4.5 |
| 羧甲基淀粉钠 | 1 |
| 二甲基硅油 | 0.1 |
| 水 | 26.9 |
制备方法：先将盐酸、乙二醇、羧甲基淀粉钠溶解于水中，形成水相；将吡唑醚菌酯和咪鲜胺溶解于二甲苯中，并加入烷基酚脂肪醇甲醛树脂聚氧乙烯醚、二甲基硅油和安全剂形成油相；将油相和水相在乳化釜中混合，即得。
实施例2
39％吡唑醚菌酯和咪鲜胺复配水乳剂，各组分及其重量份如下：
制备方法同实施例1。
实施例3
38％吡唑醚菌酯和咪鲜胺复配水乳剂，各组分及其重量份如下：
| 成分 | 重量份 |
| 吡唑醚菌酯 | 9 |
| 咪鲜胺 | 29 |
| 安全剂 | 2 |
| 二甲苯 | 15 |
| 烷基酚脂肪醇甲醛树脂聚氧乙烯醚 | 10 |
| 盐酸 | 0.5 |
| 乙二醇 | 4.5 |
| 羧甲基淀粉钠 | 1 |
| 二甲基硅油 | 0.1 |
| 水 | 28.9 |
制备方法同实施例1。
实施例4
41％吡唑醚菌酯和咪鲜胺复配水乳剂，各组分及其重量份如下：
| 成分 | 重量份 |
| 吡唑醚菌酯 | 11 |
| 咪鲜胺 | 30 |
| 安全剂 | 2 |
| 二甲苯 | 15 |
| 烷基酚脂肪醇甲醛树脂聚氧乙烯醚 | 10 |
| 盐酸 | 0.5 |
| 乙二醇 | 4.5 |
| 羧甲基淀粉钠 | 1 |
| 二甲基硅油 | 0.1 |
| 水 | 25.9 |
制备方法同实施例1。
实施例5
42％吡唑醚菌酯和咪鲜胺复配水乳剂，各组分及其重量份如下：
| 成分 | 重量份 |
| 吡唑醚菌酯 | 11 |
| 咪鲜胺 | 31 |
| 安全剂 | 2 |
| 二甲苯 | 15 |
| 烷基酚脂肪醇甲醛树脂聚氧乙烯醚 | 10 |
| 盐酸 | 0.5 |
| 乙二醇 | 4.5 |
| 羧甲基淀粉钠 | 1 |
| 二甲基硅油 | 0.1 |
| 水 | 24.9 |
制备方法同实施例1。
实施例6
40％吡唑醚菌酯和咪鲜胺复配水乳剂，各组分及其重量份如下：
| 成分 | 重量份 |
| 吡唑醚菌酯 | 10 |
| 咪鲜胺 | 30 |
| 藜芦马林碱 | 0.5 |
| 安全剂 | 2 |
| 二甲苯 | 15 |
| 烷基酚脂肪醇甲醛树脂聚氧乙烯醚 | 10 |
| 盐酸 | 0.5 |
| 乙二醇 | 4.5 |
| 羧甲基淀粉钠 | 1 |
| 二甲基硅油 | 0.1 |
| 水 | 26.4 |
制备方法同实施例1。
实施例1～6所制备的吡唑醚菌酯和咪鲜胺复配水乳剂，产品各项技术指标的检测结果如表1所示，产品热贮稳定性试验结果如表2所示。
表1 6个实施例制备产品各项技术指标的检测结果
表2 6个实施例制备产品热贮稳定性试验结果
通过表1和2可以看出，实施例1和6制备的产品在悬浮率、湿筛试验等以及热贮稳定性等方面均明显优于其他实施例所制备的产品。
二、毒理学资料
吡唑醚菌酯：大鼠急性经口LD50>5000mg/kg.急性经皮LD50>2000mg/kg.急性吸入LC50(4h)>0.3lmg/L；对兔眼睛、皮肤无刺激性。
咪鲜胺：大白鼠急性经口LD50>1600mg/kg。属低毒级。
三、吡唑醚菌酯和咪鲜胺复配水乳剂的室内生物活性(毒力)测定。
1、实验目的
旨在测定吡唑醚菌酯、咪鲜胺及二者不同比例配比对炭疽病的毒力，以判断二者不同配比对抑制炭疽病是否有增效作用。
2、试验条件
2.1供试靶标
炭疽杆菌(Bacillus anthraci)，由合肥市水基化生物新材料工程技术研究中心分离、纯化、保存并提供。
2.2培养条件
生物培养箱内培养，温度25±1℃，相对湿度85-95％。
2.3仪器设备
电子天平(感量0.1mg)、生物培养箱、直径9cm培养皿、移液管/枪、接种器、打孔器、卡尺等。
3、试验设计
3.1试材准备
将炭疽杆菌病原菌放在生化培养箱中培养，备用。
3.2药剂
吡唑醚菌酯(pyraclostrobin)原药，创新美兰(合肥)股份有限公司提供。
咪鲜胺(Prochloraz)原药，创新美兰(合肥)股份有限公司提供。
3.3药剂配制
用丙酮将实施例1-6制备的药剂稀释成5个系列质量浓度。
4、试验方法
参照《农药室内生物测定试验准则----杀菌剂》(NY/T1156.6—2006)进行。为了摸索各药剂对供试菌株的作用浓度，先进行预备实验。即将菌丝放置在含有较高和较低浓度药剂的培养基下进行培养，估算出EC50，然后再根据估算的EC50值，将培养基配成其EC50左右的不同浓度梯度的含药培养基进行培养。
本试验采用平皿菌丝生长速率法测定药剂对炭疽杆菌的毒力。具体方法如下：经转接活化的炭疽杆菌菌株用PSA培养基培养，待菌落长至培养皿四分之三大小时，用内径为5mm的打孔器从边缘打孔，打成的菌丝块作为接种体。分别将药剂母液加人灭菌融化的PSA培养基中，充分摇匀，使药剂最终浓度(按有效成分计算)达到不同浓度梯度。每皿倒入15mL左右含药培养基，设不加药为对照，每处理4个重复。移接新生长的菌丝块(直径5mm)于平板中央，后置于25℃温箱内培养2d(炭疽杆菌)、7d(炭疽杆菌)和15d(炭疽杆菌)。用十字交叉法测量菌落直径，计算各处理净生长量、菌丝生长抑制率。
式中：菌碟直径为5mm。
5、数据统计分析
将菌丝生长抑制率换算成机率值(y)，药剂浓度(μg/mL)转换成对数值(x)，以最小二乘法求得毒力回归方程(y＝a+bx)。用DPS统计软件对各单剂及不同混剂的浓度对数值和相应抑制率机率值进行回归分析，计算EC50值及95％置信限。
根据EC50计算复配剂的实测毒力指数(ATI)、理论毒力指数(TTI)和共毒系数(CTC)。
复配剂实测毒力指数(ATI)＝单剂EC50/复配剂EC50×100
复配剂理论毒力指数(TTI)＝A毒力指数×A在复配剂中含量(％)+B毒力指数×B在复配剂中含量(％)
共毒系数(CTC)＝ATI/TTI×100
根据孙云沛法计算药剂不同配比联合增效比值(CTC)，CTC≤80为拮抗作用，80＜CTC＜120为相加作用，CTC≥120为增效作用。
6、结果与分析
实施例1和6制备的水乳剂对炭疽病的联合毒力表现为明显增效作用(共毒系数分别达到170、173)，而实施例2-5制备的水乳剂对炭疽病的联合毒力仅表现为相加作用(共毒系数依次为80、85、95、90)。同时，通过实施例6的实验可以看出，在复配水乳剂中添加了少量的藜芦马林碱后，可使吡唑醚菌酯和咪鲜胺的复配联合作用进一步提升。
Claims (2)
1.一种吡唑醚菌酯和咪鲜胺复配水乳剂，其特征在于：至少由以下重量份的组分制成：
2.一种制备如权利要求1所述吡唑醚菌酯和咪鲜胺复配水乳剂的方法，其特征在于：先将盐酸、乙二醇、羧甲基淀粉钠溶解于水中，形成水相；将吡唑醚菌酯和咪鲜胺溶解于二甲苯中，并加入烷基酚脂肪醇甲醛树脂聚氧乙烯醚、二甲基硅油和安全剂形成油相；将油相和水相在乳化釜中混合，即得吡唑醚菌酯和咪鲜胺复配水乳剂。
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