CN116406662B - 一种植物源混合微乳液及其制备方法和应用 - Google Patents
一种植物源混合微乳液及其制备方法和应用 Download PDFInfo
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- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
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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
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Abstract
本发明涉及农药制备技术领域,具体公开了一种植物源混合微乳液及其制备方法和应用,通过将表面活性剂与助表面活性剂按照质量比3:1混合获得混合微乳剂,所述表面活性剂为Tween‑80或Tween‑60,所述助表面活性剂为无水乙醇,然后将混合微乳剂与油相按照质量比8‑18:2获得植物源混合微乳液,所述油相由丁香油和八角茴香油混合而成;本发明制备得到的植物源混合微乳液能够有效防治桑葚菌核病。
Description
技术领域
本发明涉及农药制备技术领域,具体涉及一种植物源混合微乳液及其制备方法和应用。
背景技术
微乳剂(microemulsion)是一种外观呈透明或半透明,粒径小且均匀的热力学稳定体系,由油相、水相、表面活性剂和助表面活性剂按照一定比例混合,自发形成(Paul andMoulik,1997)。微乳剂的表面张力很低,喷撒在植物叶片上后,能迅速铺开,待水蒸发以后,能够形成液晶相,液晶相能将农药牢固地粘附在叶表面上,使农药的利用率大大提高。此外,由于微乳剂表面张力很低,可以克服叶片表皮组织中毛细管的阻力,使有效成分更容易向叶片的内部进行渗透,能够使农药剂型的药效得到提高。
植物精油作为从植物中提取的天然有效物质,许多种植物精油的优异的抗菌能力已被证实。因其高效、低毒、环境友好等特点常作为药物的有效成分,但是由于其性质不稳定,易挥发,难溶于水,限制了植物精油的使用范围。为了增加植物精油作为植物源杀菌剂的稳定性,可以将其作成微乳剂的形式,延长植物源杀菌剂的使用期限和杀菌效果。
桑葚菌核病一般有三种类型,分别为桑葚肥大性菌核病、桑葚缩小性菌核病以及桑葚小粒性菌核病,病原依次为白杯盘菌、白井地杖菌、肉阜状杯盘菌。该病主要侵染雌花、青果及早生桑的新梢和嫩芽。孢子侵入雌花,寄生于桑果内,产生大量菌丝,果肉肿胀,呈乳白色。该病病势猛,流行频率高,极易扩大传染,并有连年暴发的特点,对桑树特别是果用桑树的危害非常大,如不及时防治,严重的可导致桑园颗粒无收,给桑农带来巨大的经济损失。目前,对于桑葚菌核病的防治效果不佳,严重影响了桑园的正常收获。
发明内容
为制备一种能防治桑葚菌核病的植物源混合微乳液,本发明提供了一种植物源混合微乳液及其制备方法和应用,本发明制备得到的混合微乳液对桑葚菌核病有防治效果。
本发明提供了一种植物源混合微乳液的制备方法,其特征在于,包括如下步骤:
S1,将表面活性剂与助表面活性剂按照质量比3:1混合获得混合微乳剂;
所述表面活性剂为Tween-80或Tween-60;
所述助表面活性剂为无水乙醇;
S2,然后将混合微乳剂与油相按照质量比8-18:2获得植物源混合微乳液;
所述油相由丁香油和八角茴香油混合而成。
进一步地,S1中,所述表面活性剂为Tween-80。
进一步地,S2中,所述混合微乳剂与油相质量比为8:2。
进一步地,S2中,所述混合精油由丁香油和八角茴香油按照质量比2:1混合而成。
本发明还提供了上述方法制备获得的植物源混合微乳液。
本发明还提供了所述的植物源混合微乳液在桑葚菌核病防治中的应用。
进一步地,所述桑葚菌核病由桑实杯盘菌引起。
与现有技术相比,本发明的有益效果在于:
1、本发明制备的植物源混合微乳液中以Tween-80为表面活性剂,所形成的微乳面积区显著大于Tween-60,乳化效果最好;助表面活性剂为无水乙醇时,能同时与两种植物精油(丁香油和八角茴香油)互溶,说明无水乙醇在作为助表面活性剂的时候可以更好地降低界面张力,调节体系黏度,有助于微乳区间的形成,满足制作混合微乳的条件。
2、本发明中的植物源混合微乳液中的油相为丁香油和八角茴香油按照质量比2:1混合获得,相比较单一使用丁香油或八角茴香油,本申请中使用丁香油和八角茴香油按照质量比2:1混合制备油相对桑葚菌核病的防治效果最佳,起到1加1大于2的效果。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
图1为丁香油与八角茴香油的化学成分分析图;
其中,图A为丁香油的总离子色谱图;
图B为八角茴香油的总离子色谱图。
图2为Tween-80(A)、Tween-60(B)、Tween-20(C)的微乳伪三元相图;
其中,图A为Tween-80的微乳伪三元相图;
图B为Tween-60的微乳伪三元相图;
图C为Tween-20的微乳伪三元相图。
图3为不同Km值的微乳伪三元相图;
其中,图A为Km值为1:1的微乳伪三元相图;
图B为Km值为2:1的微乳伪三元相图;
图C为Km值为3:1的微乳伪三元相图;
图D为Km值为4:1的微乳伪三元相图。
图4为丁香微乳液、八角茴香微乳液与混合微乳液外观图;
其中,从左到右依次为丁香微乳液、八角茴香微乳液与混合微乳液外观图。
具体实施方式
下面对本发明的具体实施方式进行详细描述,但应当理解本发明的保护范围并不受具体实施方式的限制。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动的前提下所获得的所有其他实施例,都属于本发明保护的范围。本发明各实施例中所述实验方法,如无特殊说明,均为常规方法,下述实施例中所用的材料、试剂等,如无特殊说明,均可从商业途径得到。
实施例1:一种植物源混合微乳液及其制备方法和应用。
一、材料
1、试验材料
主要试剂:八角茴香油、丁香油(上海源叶生物有限公司);Tween-80、Tween-60、Tween-20(成都市科隆化学品有限公司);无水乙醇,乙二醇、甘油。
二、实验方法
1、精油成分的GC-MS分析
(1)八角茴香油气相色谱条件:
采用岛津GCMS-QP2010气质联用仪;色谱柱:Rtx-5ms(30m×0.25mm×0.25um);进样口温度250℃;载气:氦气(He);柱流速:1mL/min;进样量0.2μL;分流比10:1;程序升温:初始柱温60℃,保持1min,5℃/min升到240℃,保持5min。
八角茴香油质谱条件:
电子轰击(EI)离子源,电离能量:70eV;离子源温度:230℃;接口温度:250℃;四级杆温度:150℃;质量扫描范围:30~500amu;检索谱库:NIST08,最后用峰面积计算各成分占的百分比含量。
丁香油气相色谱条件:
采用岛津GCMS-QP2010气质联用仪;色谱柱:Rtx-5ms(30m×0.25mm×0.25um);进样口温度270℃;载气:氦气(He);柱流速:1mL/min;进样量1μL;分流比40:1;程序升温:初始柱温70℃,保持1min,5℃/min升到190℃,保持15min。
(2)丁香油质谱条件:
电子轰击(EI)离子源,电离能量:70eV;离子源温度:230℃;接口温度:230℃;四级杆温度:150℃;质量扫描范围:35~500amu;检索谱库:NIST08,最后用峰面积计算各成分占的百分比含量。
2、植物源混合微乳液的制备和优化
在制备植物源混合微乳液的过程中,各组分之间的比值均为其质量之比。
(1)助表面活性剂的初步筛选
在5mL带有刻度的EP管中分别加入1.0g植物精油(丁香油和八角茴香油),分别向其中加入3.0g的备选试剂(无水乙醇、1,2-丙二醇、丙三醇、甘油),用高速漩涡震荡仪震荡混匀之后,静置观察其混合情况,从中筛选出适合的助表面活性剂。
(2)微乳伪三元相图的绘制
先固定油相和表面活性剂的比值,之后往体系中滴加水相来计算各组分的含量,并绘制伪三元相图:根据筛选的微乳基本处方,将表面活性剂与助表面活性剂按照一定质量比(Km)混合制成混合微乳剂(Smix)。用磁力搅拌器均匀混合后,按其与油相质量比为9:1,8:2,7:3,6:4,5:5,4:6,3:7,2:8,1:9混合获得植物源混合微乳液。随后在油相中一边搅拌一边逐渐滴加蒸馏水。肉眼观察滴加过程中液体体系由清变浊或由浊变清的瞬间,记录临界点的加水量,确定微乳区界限。
按照水相、油相、混合微乳剂(Smix)作为伪三元相图的三个顶点,根据各组分在临界点的质量百分比利用Origin2021软件绘制伪三元相图。
(3)表面活性剂的选择
分别用Tween-80,Tween-60,Tween-20作为表面活性剂,与助表面活性剂(无水乙醇)配成Km=3:1比例的混合微乳剂,参照上述的方法绘制微乳伪三元相图。
(4)表面活性剂与助表面活性剂配比(Km)的选择
以Tween-80为表面活性剂,无水乙醇为助表面活性剂。按照一定的质量比(Km=4:1,3:1,2:1,1:1)混合,参照上述的方法绘制微乳伪三元相图。
3、微乳基本性质考察
(1)微乳外观及类型鉴别
微乳制备完成后,依据标准,肉眼观察根据处方研制的微乳液,是否均一、澄清、蒸馏水稀释后仍为透明或近似透明的稳定液体体系。不会分层或破乳等,视为合格。
染色法鉴定微乳类型:吸取相同体积的两份微乳样品于试管中,各取一滴苏丹红IV染料溶液和亚甲基蓝染料溶液分别滴入试管,观察两种染料的扩散速度。若亚甲基蓝染料在微乳中的扩散速度大于苏丹红IV染料,则制备出的微乳类型为O/W型,如苏丹IV染料的扩散速度大于亚甲基蓝染料,则制备的微乳类型为W/O型。
(2)微乳的粒径及分布考察
采用NanoBrook Omni纳米粒度分析仪测定微乳的粒径大小及分布。为避免多重散射影响观察结果,乳液均经水稀释50倍后再进行测定。
4、微乳稳定性检测
(1)微乳稳定性检测
参考农药乳油国家标准规定的测试方法进行乳液稳定性检测。用342mg/L的标准硬水将待测样品稀释,于20℃下静置30min,观察样品稀释后外观情况,若任能保持透明状态、无固体物沉淀或油状物的悬浮,并且能与水在任何比例条件下混合,则视乳液为稳定状态。
(2)微乳离心稳定性检测
取适量微乳置于2.5mL离心管中,4000r/min离心20min,观察后微乳的颜色、外观变化。
三、结果分析
1、丁香油与八角茴香油的化学成分分析
利用GC-MS技术对丁香油和八角茴香油进行成分分析,总离子色谱图如图1所示。丁香油气相色谱共检测出挥发性成分5种(图1的图A),主要成分及含量见表1。其中含量最高的是丁香酚(85.54%)、石竹烯(11.96%)、α-石竹烯(2.34%)三种物质,占总量的99.84%。八角茴香气相色谱检测出挥发性成分2种(见表2),其中含量最高的化合物是反式茴香脑(图1的图B),占总含量的99.98%。
表1丁香油的主要成分
表2八角茴香油的主要成分
2、精油微乳液的制备和优化
(1)助表面活性剂的初步筛选
微乳中助表面活性剂通过调节表面活性剂的HLB值,降低液面张力,形成微乳球状分子所需的液面曲率,提高界面流动性,可以大大提高乳化效率。本试验选用无水乙醇、1,2-丙二醇、丙三醇、甘油作为助表面活性剂进行优选试验结果如表3所示。结果显示,只有无水乙醇能同时与两种植物精油(丁香油和八角茴香油)互溶,说明无水乙醇在作为助表面活性剂的时候可以更好地降低界面张力,调节体系黏度,有助于微乳区间的形成,满足制作混合微乳的条件。因此选择无水乙醇作为助表面活性剂。
表3精油在溶剂中的溶解情况
(2)表面活性剂的选择
表面活性剂是构成微乳剂的物质之一,通过降低界面张力促进微乳形成。Tween系列表面活性剂因其安全、刺激小、价格低廉、乳化效果显著等优势,被广泛应用于食品、化妆品以及医药等工业领域。本试验选用Tween-80、Tween-60、Tween-20作为研究对象,以选出较优的表面活性剂。以丁香八角混合精油(质量比=2:1)作为油相,无水乙醇为助表面活性剂。按照上述方法,当Km=3:1时,可作出不同表面活性剂微乳的伪三元相图(图2)。由图2可知Tween-20在该体系中不能形成有效的微乳区域(图2的图C),而Tween-80所形成的微乳面积区大于Tween-60(图2的图A和图B)。因此选取乳化效果最好的Tween-80作为表面活性剂。
(3)表面活性剂与助表面活性剂配比(Km)的选择
表面活性剂与助表面活性剂的比值(Km)对乳化体系的制备至关重要,不同的乳化体系中,Km的值也有区别,Km的比值不同会影响微乳形成的效果。本试验选择乳化效果较好的Tween-80为表面活性剂,无水乙醇为助表面活性剂,按Km比值1:1、2:1、3:1、4:1的比例进行混合,绘制微乳伪三元相图,考察不同Km的值对微乳形成面积大小影响。
如图3所示,随着Km比值逐渐增大,微乳区面积也在逐渐增大,至Km=3:1时微乳区面积达到最大值,之后微乳区面积有所减小。表明在一定量助表面活性剂存在的情况下,表面活性剂比例越高,形成微乳的能力越好。而当Km值超过3:1后,所形成微乳区域减小,可能是由于较高浓度的表面活性剂缺少助表面活性剂的助乳化作用而导致体系形成微乳能力的降低。故确定选用Km=3:1作为最佳的Km值。
(4)混合微乳液优化
在构建混合微乳剂伪三元相图过程中,已经确定表面活性剂为Tween-80,助表面活性剂为无水乙醇,两者比值Km=3:1。当混合微乳剂Smix:油相的比值在9:1、8:2以及7:3时,所制成的混合微乳液为清澈透明的微乳液,当比值低于7:3时,微乳***不稳定,易产生浑浊。其中比值9:1与8:2的精油微乳液稳定性良好,稀释后仍呈现出澄清透明状态,显示出良好的稀释性。因微乳载药量的考量,最终选择Smix:油相=8:2作为最终的混合微乳液配方。油相选择单一八角茴香油或丁香油,鉴于对桑葚菌核病的防治效果,优选丁香油:八角茴香油按照质量比2:1的混合物做为油相,选择购买自中国典型培养物保藏中心的桑实杯盘菌,保藏编号为CCTCC AF 2014019,抑菌效果见表4。
表4八角茴香油和丁香油复配物对桑实杯盘菌的抑制效果
注:“十"表示有菌生长,“一”表示无菌生长;MICA和MICB分别表示八角茴香油和丁香油对桑实杯盘菌的MIC值。
3、混合微乳液基本性质测定结果
(1)混合微乳液外观及类型鉴别
按照配方制作成的微乳如图4所示,制备出微乳均澄清透明,带有淡蓝色乳光。同时向微乳中滴加亚甲基蓝染料与苏丹IV染料后,亚甲基蓝染料在微乳中的扩散速度明显大于苏丹IV染料,故可以判定本试验制备出的微乳属O/W型微乳。
(2)混合微乳液的粒径及分布考察
采用激光粒度仪测定三种微乳的平均粒径及分布,结果如表5所示。三种精油微乳粒径均小于100nm,且粒径分布离散程度较小,符合微乳液的定义。
表5微乳液粒径大小及分布
(2)微乳稳定性检测
对微乳液进行10倍、100倍稀释,结果发现,稀释后的微乳液仍呈现出澄清透明状态,显示出良好的稀释性。
(3)微乳稳定性检测
将所测样品在4000r/min的条件下离心20min后,取样观察,所有样品外观均透明均一,未有分层现象出现,结果表明微乳稳定性较好。
尽管已描述了本发明的优选实施例,但本领域内的技术人员一旦得知了基本创造性概念,则可对这些实施例作出另外的变更和修改。所以,所附权利要求意欲解释为包括优选实施例以及落入本发明范围的所有变更和修改。
显然,本领域的技术人员可以对本发明进行各种改动和变型而不脱离本发明的精神和范围。这样,倘若本发明的这些修改和变型属于本发明权利要求及其等同技术的范围之内,则本发明也意图包含这些改动和变型在内。
Claims (5)
1.一种植物源混合微乳液的制备方法,其特征在于,包括如下步骤:
S1,将表面活性剂与助表面活性剂按照质量比3:1混合获得混合微乳剂;
所述表面活性剂为Tween-80或Tween-60;
所述助表面活性剂为无水乙醇;
S2,然后将混合微乳剂与油相按照质量比9:1或8:2混合获得植物源混合微乳液;
所述油相由丁香油和八角茴香油按照质量比2:1混合而成。
2.根据权利要求1所述的植物源混合微乳液的制备方法,其特征在于,S1中,所述表面活性剂为Tween-80。
3.一种权利要求1-2所述的制备方法制备获得的植物源混合微乳液。
4.一种权利要求3所述的植物源混合微乳液在桑葚菌核病防治中的应用。
5.根据权利要求4所述的植物源混合微乳液在桑葚菌核病防治中的应用,其特征在于,所述桑葚菌核病由桑实杯盘菌引起。
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