CN105724441B - 一种菊芋叶片二氯甲烷提取物乳化物及其制备方法和应用 - Google Patents
一种菊芋叶片二氯甲烷提取物乳化物及其制备方法和应用 Download PDFInfo
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- A01N65/08—Magnoliopsida [dicotyledons]
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- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
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- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/22—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing ingredients stabilising the active ingredients
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Abstract
本发明公开了一种菊芋叶片二氯甲烷提取物乳化物及其制备方法和应用。菊芋叶片二氯甲烷提取物乳化物配方为菊芋叶片二氯甲烷提取物浸膏5％，溶剂8～20％，乳化剂组合9～12％，助溶剂或助表面活性剂9～10％，余量为水，配方中所有物质的百分含量之和为100％；其中所述的溶剂选自无水乙醇，所述的乳化剂组合选自壳聚糖/DBS‐Na、OP‐10/DBS‐Na、NP‐10/DBS‐Na中的一种；所述的助溶剂或助表面活性剂选自甲醇和环己酮。本发明是从菊芋叶片中浸提出粗提取物用来制备二氯甲烷乳化物，并通过对配方的优化，成功将菊芋叶片二氯甲烷提取物制备成性质稳定的乳化物。
Description
技术领域
本发明属于绿色农药制剂领域，涉及一种菊芋叶片二氯甲烷提取物乳化物及其制备方法和应用。
背景技术
菊芋又名洋姜，是菊科、向日葵属宿根性草本植物，它的原产地来自北美洲，到十七世纪传入欧洲，之后才传入中国。菊芋适应性强，耐寒、耐旱、耐贫瘠。菊芋叶片大多秋季开花，呈黄色形如菊，花期一般在8～10月。叶基部对生，叶面粗糙，叶背有柔毛，边缘锯齿，绿色。菊芋叶片可以作为解热、镇痛、抗炎和抗痉挛的药物，治疗骨折、皮肤创伤、疼痛和肿胀等。此外，菊芋的业叶片还具有抗氧化、抗细菌、抗真菌和抗癌的活性。目前已发现的菊芋叶片中活性物质有酚类、黄酮类、总糖和总蛋白等主要化合物，是待开发的能源植物之一。研究较多的是酚类物质，有10种属于绿原酸类(CGAS)化合物，包括3种绿原酸异构体、4种二咖啡酰奎奎尼酸异构体、咖啡酸、P-香豆酰奎尼酸、阿魏酰奎尼酸，还有其他四种化合物，分别是异鼠李素-O-葡萄糖苷、咖啡酰葡萄糖、山奈酚葡萄糖醛酸苷、山奈酚-3-O-葡萄糖苷。菊芋叶片可以利用现在科学技术开发新型无公害的杀虫剂和杀菌剂，有利于保护人类的生存环境。
随着社会的发展和科学技术的提高，绿色农药乳剂已出现在人们的视角中，而我国对菊芋叶片乳剂方面的研究几乎是空白，有较大的研究空间待于挖掘。
发明内容
本发明的目的是提供一种菊芋叶片二氯甲烷提取物乳化物。
本发明的另一目的是提供该菊芋叶片二氯甲烷提取物乳化物的制备方法。
本发明的又一目的是提供该菊芋叶片二氯甲烷提取物乳化物的应用。
本发明的目的可通过以下技术方案实现：
一种菊芋叶片二氯甲烷提取物乳化物，菊芋叶片二氯甲烷提取物乳化物配方为菊芋叶片二氯甲烷提取物浸膏5％，溶剂8～20％，乳化剂组合9～12％，助溶剂或助表面活性剂9～11％，余量为水，配方中所有物质的质量百分含量之和为100％；其中所述的溶剂选自无水乙醇，所述的乳化剂组合选自壳聚糖/DBS-Na、OP-10/DBS-Na、NP-10/DBS-Na中的一种；所述的助溶剂 或助表面活性剂选自甲醇和环己酮。
其中，乳化剂组合选自壳聚糖/DBS-Na时，壳聚糖与DBS-Na的质量比优选为3:1，乳化剂组合选自OP-10/DBS-Na时，OP-10与DBS-Na的质量比为3:1.6～1，乳化剂组合选自NP-10/DBS-Na时，NP-10与DBS-Na的质量比为3:1。
所述的甲醇和环己酮的质量比为0.8～1:1。
所述的菊芋叶片二氯甲烷提取物乳化物配方进一步优选为菊芋叶片二氯甲烷提取物浸膏5％，DBS-Na 2.5～4％，OP-10 7.5％，乙醇10～20％，甲醇4～5％，环己酮6％，余量为水，配方中所有物质的百分含量之和为100％。
所述的菊芋叶片提取物浸膏优选通过以下方法提取：菊芋叶片放于容器中然后倒入是70％乙醇，菊芋叶片与70％乙醇的质量体积比为1:6～4，浸提25～30天，每天搅拌3～5次，每次2～5分钟；乙醇提取液用真空抽气装置抽滤，滤出液用旋转蒸发仪旋蒸，旋蒸除去乙醇；旋蒸得出的浓缩液再经石油醚、二氯甲烷萃取，分别得到石油醚萃取液、二氯甲烷萃取液，二氯甲烷萃取液旋蒸去水，最后得到菊芋叶片二氯甲烷提取物浸膏。
所述的水的硬度，以碳酸钙浓度计优选小于等于342mg/L。
微乳剂质量检测显示乳液稳定性符合试验要求、水质的硬度在0～342mg/L(以碳酸钙浓度计)、热(54土2℃)贮平均分解率仅在6.7％，表明乳剂热贮性稳定，其pH值范围为5～8。
本发明所述的菊芋叶片二氯甲烷提取物乳化物的制备方法，包括以下步骤首先制备二氯甲烷提取物浸膏，然后按照配方中二氯甲烷提取物浸膏、溶剂、乳化剂组合、助溶剂或助表面活性剂和水的百分含量逐一向二氯甲烷提取物浸膏中添加溶剂、乳化剂组合、助溶剂或助表面活性剂和水并搅拌均匀，用酸或者碱调整菊芋叶片二氯甲烷提取物乳化物pH为5～8即得所述的菊芋叶片二氯甲烷提取物乳化物。
本发明所述的菊芋叶片二氯甲烷提取物乳化物在抑制小麦赤霉病菌、水稻稻瘟病菌和板栗炭疽病菌中的应用。
本发明所述的菊芋叶片二氯甲烷提取物乳化物在制备绿色农药中的应用。
有益效果：本发明所提供的南菊芋1号叶片二氯甲烷提取物乳化物的制备方法，具有如下优点 和积极效果：
1)本发明是从菊芋叶片中浸提出粗提取物用来制备二氯甲烷乳化物，并通过对配方的优化，成功将菊芋叶片二氯甲烷提取物制备成性质稳定的乳化物。
2)本发明适用于多个菊芋品种，以菊芋叶片为原料均可用本方法得到具有乳剂活性的粗提物。
3)原材料为菊芋叶片废弃物，比较经济。
4)菊芋叶片提取物制备乳化物，不同于传统化学乳剂，具备更加环保的优点。
5)试验中用到的旋转蒸发仪能快速、温和的对菊芋浓缩液进行旋蒸，不会沸腾损失浓缩液，大大的增加了浓缩效率。
附图说明
图1乳液稳定性考察结果
图2二氯甲烷提取物乳化物对小麦赤霉病菌生长的抑制作用
A、B为对照组小麦赤霉病菌菌丝生长图；C、D为处理组小麦赤霉病菌菌丝生长图。
图3二氯甲烷提取物乳化物对水稻稻瘟病菌生长的抑制作用
A、B为对照组水稻稻瘟病菌菌丝生长图；C、D为处理组水稻稻瘟病菌菌丝生长图。
图4二氯甲烷提取物乳化物对板栗炭疽病菌生长的抑制作用
A、B为对照组板栗炭疽病菌菌丝生长图；C、D为处理组板栗炭疽病菌菌丝生长图。
具体实施方式
下述实施例中所使用的实验方法如无特殊说明，均为常规方法。
下述实施例中所使用的石油醚(60～90℃)、二氯甲烷均为分析纯，购自上海化学试剂有限公司；旋转蒸发仪(RE-501型)购自南京金正教学仪器有限公司；其他材料、试剂等如无特殊说明，也均可从商业途径得到。
实施例1：
方法中所使用的菊芋品种为南菊芋1号，由南京农业大学资环学院海洋滩涂资源实验室提供，栽种于江苏省盐城大丰市金海农场，9～11月份收取菊芋废弃物叶片，置于105℃烘箱中15min杀青，继而转为75℃，1～2d烘干，之后取出贮存备用。
1)菊芋叶片放于容器中然后倒入是70％的乙醇(w/v比例为1:4)，浸提25天，每天搅拌3次，每次5分钟；乙醇提取液用真空抽气装置抽滤，滤出液用旋转蒸发仪旋蒸，旋蒸除去乙醇；旋蒸得出的萃取液再经石油醚、二氯甲烷萃取，分别得到石油醚萃取液、二氯甲烷萃取液，二氯甲烷萃取液旋蒸去水，最后得到目标浸提物：菊芋叶片二氯甲烷提取物浸膏。
2)溶剂品种的选择
在具塞试管中分别加入0.5g菊芋叶片提取物浸膏，分别向其中加入1.5mL无水乙醇、无水甲醇、甲醇、乙酸乙酯、N,N-二甲基甲酰胺、二甲基亚砜、苯、二甲苯溶剂，充分振荡、摇晃后,观察常温(25℃)溶解现象，其中，无水乙醇对水饱和正丁醇浸膏溶解性能最好，因此，选择无水乙醇作为溶剂。
3)溶剂用量的选择
在具塞试管中分别加入0.5g菊芋叶片提取物浸膏，分别加入0.5mL、1mL、1.5mL、2mL上述八种备选常用溶剂，充分振荡、摇晃后,观察常温(25℃)溶解现象，确定最佳用量是2ml。
4)乳化剂预选结果
在具塞试管中分别加入0.5g菊芋叶片提取物浸膏溶液，按照0.4、0.25、0.1g三个量加入DBS-Na，随后再向各试管分别按照0.5、0.75g两个量加入各种非离子表面活性剂，在70℃的水浴中混匀，最后用去离子水补足10mL，混匀。将制备好的样品在0-60℃的范围内进行温度观察，在某个温度能够出现透明或半透明现象的体系进入下一轮筛选，其余的体系不再进行考察。
由下表中可以看出，能够出现透明的体系共4个，涉及的乳化剂组合有壳聚糖/DBS-Na、OP-10/DBS-Na、NP-10/DBS-Na，确定这3个乳化剂组合进入下一轮筛选。
5)助溶剂或助表面活性剂的筛选
通过甲醇、环己酮、正丁醇、乙二醇、异丙醇这几种溶剂在不同乳化剂体系中对透明温度范围的影响，筛选出具有较好温度适应性的助表面活性剂。
从下表中可以看出，甲醇和环己酮在所选的乳化剂体系中温度范围最宽，而正丁醇、乙二醇和异丙醇在所选的乳化剂体系中只有很窄的温度范围。
6)透明温度范围
由下表中可以看出，在DBS-Na/OP-10体系中加入不同量甲醇和环己酮体系的透明温度范 围，当甲醇和环己酮的加入量分别为0.4g和0.6g时，可获得0～50℃的透明温度范围。
经过以上筛选，得到一种透明温度范围符合微乳剂技术要求的配方组成：菊芋叶片提取物浸膏5％，DBS-Na 2.5～4％，OP-107.5％，乙醇10-20％，甲醇4～5％，环己酮6％，余量为水，配方中所有物质的百分含量之和为100％。
实施例2微乳剂质量检测
实施例1制备的菊芋叶片提取物浸膏5％，DBS-Na 2.5％，OP-107.5％，乙醇12％，甲醇4％，环己酮6％，余量为水，各原料总质量百分含量为100％。
按照配方中菊芋叶片二氯甲烷提取物浸膏、溶剂、乳化剂组合、助溶剂或助表面活性剂和水的百分含量逐一向菊芋叶片二氯甲烷提取物浸膏中添加溶剂、乳化剂组合、助溶剂或助表面活性剂和水并搅拌均匀，用酸或者碱调整菊芋叶片二氯甲烷提取物乳化物pH为5～8即得所述的菊芋叶片二氯甲烷提取物乳化物。
水质的选择
筛选出342mg/L(以碳酸钙浓度计)以下不同硬度的水质，微乳剂外观状态及乳液稳定性无差异结果见下表。
乳液稳定性
将二氯甲烷乳剂用342mg/L(以碳酸钙浓度计)硬水稀释200倍，其初始外观为透明乳状液，无油状物或固体沉淀(如图1A)，经放置数小时后透明度下降，24小时后变为粗乳状液(如图1B)。
热贮稳定性
将二氯甲烷乳剂在54±2℃的条件下贮存两周，对五组(水质选择)中二氯甲烷浸膏的热贮分解率进行测定，其分解率如下：6.6％、5.7％、6.2％、5.2％、5.0％，平均5.7％，表明样品具有很好的热贮稳定性。
pH值
由下表可以看出，有效成分只有在pH 5～8时热贮分解率在8％以下，过酸或过碱都不利于有效成分的贮存。因此，规定制剂的PH值范围为5-8。
菊芋叶片二氯甲烷提取物乳化物的制备在菌种上的应用
培养菌种(小麦赤霉病菌、稻瘟病菌、板栗炭疽病菌)，接种，每种菌种三次重复，插平板24h后，每隔12h观察(直到得到平板物)，固定后进行扫描电镜观察。
1.二氯甲烷提取物乳化物对小麦赤霉病菌生长的抑制作用，对照组图2(A、B)菌丝粗细均勻细长，圆润饱满，生长点表面光滑无异常；处理组图2(C、D)菌丝形态发生明显的变化，菌丝断裂、老化、生长点脱落，局部凹陷并出现干瘪现象。
2.二氯甲烷提取物乳化物对水稻稻瘟病菌生长的抑制作用，对照组图3(A、B)菌丝生长粗细长短均匀，表面光滑饱满，生长无异常；处理组图3(C、D)菌丝形态发生明显的变化，菌丝粗细长短不一，生长点脱落严重，出现严重的干瘪及老化现象。
3.二氯甲烷提取物乳化物对板栗炭疽病菌生长的抑制作用，对照组图4(A、B)菌丝生长均匀饱满，表面光滑；处理组图4(C、D)菌丝大小不一，菌丝凹陷，干瘪现象严重。
Claims (7)
1.一种菊芋叶片二氯甲烷提取物乳化物，其特征在于菊芋叶片二氯甲烷提取物乳化物配方为菊芋叶片二氯甲烷提取物浸膏5%，DBS-Na 2.5~4%，OP-10 7.5%，乙醇8~20%、甲醇4~5%，环己酮6%，余量为水，配方中所有物质的百分含量之和为100%。
2.根据权利要求1所述的菊芋二氯甲烷提取物乳化物，其特征在于所述的菊芋叶片提取物浸膏通过以下方法提取：菊芋叶片放于容器中然后倒入是70%乙醇，菊芋叶片与70%乙醇的质量体积比为1:6-4，浸提25-30天，每天搅拌3-5次，每次2-5分钟；乙醇提取液用真空抽气装置抽滤，滤出液用旋转蒸发仪旋蒸，旋蒸除去乙醇；旋蒸得出的浓缩液再经石油醚、二氯甲烷萃取，分别得到石油醚萃取液、二氯甲烷萃取液，二氯甲烷萃取液旋蒸去水，最后得到菊芋叶片二氯甲烷提取物浸膏。
3.根据权利要求1所述的菊芋叶片二氯甲烷提取物乳化物，其特征在于所述的水的硬度，以碳酸钙浓度计小于等于342mg/L。
4.根据权利要求1所述的菊芋叶片二氯甲烷提取物乳化物，其特征在于菊芋叶片二氯甲烷提取物乳化物的pH为5~8。
5.根据权利要求1~4中任一项所述的菊芋叶片二氯甲烷提取物乳化物，其特征在于所述的乳化物通过以下方法制备得到：首先制备菊芋叶片二氯甲烷提取物浸膏，然后按照配方中菊芋叶片二氯甲烷提取物浸膏、溶剂、乳化剂组合、助溶剂或助表面活性剂和水的百分含量逐一向二氯甲烷提取物浸膏中添加溶剂、乳化剂组合、助溶剂或助表面活性剂和水并搅拌均匀，用酸或者碱调整菊芋叶片二氯甲烷提取物乳化物pH为5~8即得所述的菊芋叶片二氯甲烷提取物乳化物。
6.权利要求1~4中任一项所述的菊芋叶片二氯甲烷提取物乳化物的制备方法，其特征在于包含以下步骤：首先制备菊芋叶片二氯甲烷提取物浸膏，然后按照配方中菊芋叶片二氯甲烷提取物浸膏、溶剂、乳化剂组合、助溶剂或助表面活性剂和水的百分含量逐一向二氯甲烷提取物浸膏中添加溶剂、乳化剂组合、助溶剂或助表面活性剂和水并搅拌均匀，用酸或者碱调整菊芋叶片二氯甲烷提取物乳化物pH为5~8即得所述的菊芋叶片二氯甲烷提取物乳化物。
7.权利要求1所述的菊芋叶片二氯甲烷提取物乳化物在制备抑制小麦赤霉病菌、水稻稻瘟病菌和板栗炭疽病菌的制剂中的应用。
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| CN101849555A (zh) * | 2010-06-30 | 2010-10-06 | 中国热带农业科学院香料饮料研究所 | 假连翘杀菌水乳剂及其制备方法 |
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| CN101849555A (zh) * | 2010-06-30 | 2010-10-06 | 中国热带农业科学院香料饮料研究所 | 假连翘杀菌水乳剂及其制备方法 |
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