CN1194617C - 孜然杀菌剂及其制备方法 - Google Patents
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Abstract
本发明公开了一种利用植物——孜然为原料制备的杀菌剂及其方法，采用孜然(Cuminum cyminum L.)的根、茎、叶、种子为原料，其特征在于，将上述原料用乙酸己酯溶剂提取，提取液经浓缩得提取物，提取物再和溶剂、农药助剂配制成孜然杀菌乳油或微乳剂。本发明的孜然杀菌剂对环境安全，孜然杀菌剂中的活性化合物是天然存在的物质，来源于自然，在长期的进化过程中已形成了其固有的参与能量与物质循环代谢途径，所以施用于环境中或植物上，无残留，不会引起生物富集；对非靶标生物相对安全；对植物病原菌的作用机理不同于常规农药，使用后病原菌不易对其产生抗药性，对病原菌对常规杀菌剂的抗药性也有延缓作用。
Description
一.技术领域
本发明属于农林业领域，具体涉及农药制备及加工领域，特别涉及一种利用植物——孜然为原料制备的杀菌剂及其制备方法。
二.背景技术
孜然(Cuminum cyminum L.)为伞形科孜然芹属1年生2年生草本植物，我国主要产于新疆地区和甘肃河西走廊。株高20～40cm，全株(除果实外)光滑无毛；叶片3出或2回羽状复叶，全裂，末回裂片狭线形，长1.5～5.0cm，宽0.3～0.5mm；复伞形花序，多呈二歧式分枝，伞形花序直径2～3cm，小伞形花序，通常有7花，花瓣粉红色或白色，长圆形，顶端微缺有内折的小舌片，花株基部圆锥状；花柱短，叉开，柱头头状；分生果长圆形，两端狭长，长6mm，宽1.5mm，密被白色刚毛，果实千粒重2～3g。孜然芹喜冷凉气候，较耐旱，适应性强，对土壤要求不严格，一般以沙土壤为好。
我国新疆是国内孜然的最主要产地，当地维吾尔族、回族、克尔克孜族、哈萨克族等各族群众将其果实研成粉末作调料，尤其常用于烧烤肉食中。其果实也可入药，治疗消化不良和胃寒腹痛等症；能增加孕妇的乳汁，减少作呕；也可用作敷剂，减轻患者的肿胀。孜然也是维吾尔族人经常饮用的药茶中的一种重要配料。在西方，主要用于兽医医药上，作为排除胃肠气胀剂。从孜然的种子中可提取孜然油(又称枯茗油，Cumin oil)，它做为一种天然植物香料，已被FEMA、FDA等世界性学会组织和机构确认，可大量用于食品、烟草香精以及部分化妆品等日用香精中。除此之外，在许多文章中报道，孜然油具有抵抗各种病原真菌和细菌的作用。Atta-ur-Rahman及其合作者曾报道孜然油对P.boydi和A.flavus有一定的抑菌作用。另外，其精油也常用作消毒剂、防腐剂使用。而孜然对植物病原菌的抑制作用还未有全面***的报道。
三.发明内容
根据上述孜然的一些基本特性，本发明的目的在于提供一种利用孜然为原料制备的杀菌剂及其方法。
为了实现上述目的，申请人通过对孜然抑制各种植物病原菌作用的深入研究，发现了孜然全株的乙酸己酯提取物，对小麦赤霉病菌(Gibberella zeae)、玉米大斑病菌(Exserohilum turcicurn)、辣椒疫霉病菌(Phytoph thora capsicileaonian)、苹果炭疽病菌(Goloetotrichum gloeosphorivides)、番茄灰霉病菌(Botrytis cinerea)和小麦白粉病菌(Blumeria graminisr)等植物病原菌在离体条件下表现出较高的抑制作用，在活体条件下，对作物有很好的保护作用。从孜然的特性可知，其对人、畜、环境无毒、无污染，符合农药发展的方向，有望被开发成一种无公害的植物源杀菌剂。
本发明所采取的技术方案是：该孜然杀菌剂采用用孜然(Cuminum cyminumL.)的根、茎、叶、种子为原料，其特点是，将上述原料用乙酸己酯溶剂提取，提取液经浓缩得提取物，提取物再和溶剂、农药助剂配制成孜然杀菌乳油或微乳剂。
孜然杀菌剂乳油的各组份重量百分比为：
孜然提取物 50％～70％
溶剂 20％～50％
农药助剂 10％～20％
孜然杀菌微乳剂的各组份重量百分比为：
孜然提取物 10％～30％
溶剂 10％～20％
水 30％～50％
农药助剂 10％～20％
上述的孜然杀菌剂的制备方法是：
A.将干燥的孜然根、茎、叶及种子粉碎，过40目筛；
B.用4倍于孜然粉碎物重量的乙酸己酯，在回流条件下提取，提取温度70～80℃，提取时间8h；
C.用真空浓缩的方法，将孜然提取物浓缩至与孜然原料粉碎物等重，得孜然提取物；
D.在反应釜中，按杀菌乳油配比量依次加入各成份，搅拌均匀即可得孜然杀菌乳油；
E.先将孜然提取物，农药助剂溶解于溶剂中，在40℃～50℃，高速搅拌情况下将所得溶剂滴加入蒸馏水中，恒温搅拌1h，即得孜然杀菌微乳剂。
本发明的孜然杀菌剂和现在常用的杀菌剂相比，有如下特点：
1.对环境安全 孜然杀菌剂中的活性化合物是天然存在的物质，来源于自然，在长期的进化过程中已形成了其固有的参与能量与物质循环代谢途径，所以施用于环境中或植物上，无残留，不会引起生物富集；
2.对非靶标生物相对安全；
3.对植物病原菌的作用机理不同于常规农药，使用后病原菌不易对其产生抗药性，对病原菌对常规杀菌剂的抗药性也有延缓作用。
四、具体实施方式
为了更清楚的理解本发明以及本发明药剂的药效，以下通过发明人给出的依本发明技术方案所完成的如下实施例对本发明作进一步的详细描述，这些仅是本发明较好的实施例，但不限于这些实施例。
实施例1：孜然提取物的制备
将干燥的孜然根、茎、叶及种子粉碎，过40目筛。称取孜然粉碎物100kg于回流提取釜中，再加入400kg乙酸己酯溶液，在70℃～80℃温度下，回流提取8h，过滤得提取液。将提取液浓缩至100kg，即得孜然提取物。
实施例2：孜然杀菌乳油的制备
称取孜然提取物50kg，用甲醇40kg溶解，在搅拌下加入壬基酚聚氧乙烯醚9kg和十二烷基苯磺酚钙1kg，搅拌均匀，即得100kg孜然杀菌乳油。
实施例3：孜然杀菌微乳剂的制备
称取孜然提取物30kg，和15kg壬基酚聚氧乙烯醚磷酸酯，溶于15kg乙醇中，将以上溶液在匀质机中加热至43℃，高速搅拌下滴加无离子水40kg；滴加完毕，再搅拌45分钟，冷却，即得孜然杀菌微乳剂。
试验实施例1：测定孜然乙酸己酯提取物对植物病原菌的抑制活性
本实验在离体条件下，测定了孜然乙酸己酯提取物对植物病原菌的抑制活性，实验方法和实验结果如下：
1.供试菌种
小麦赤霉病菌(Gibberella zeae)、玉米大斑病菌(Exserohilumturcicurn)、辣椒疫霉病菌(Phytophthora capsici leaonian)、苹果炭疽病菌(Goloetotrichum gloeosphorivides)和番茄灰霉病菌(Botrytis cinerea)，均由西北农林科技大学植物病理研究所提供。
2.试验方法
将上述孜然杀菌乳油采用菌丝生长速率法和孢子萌发法对供试病原菌进行离体生物活性测定，按下列公式计算抑制率：
3.试验结果
用生长速率法测定了孜然杀菌乳油对供试病原菌的毒力，从而求出孜然提取物对供试病原菌的毒力，结果见表1。
表1孜然提取物对病原菌的毒力测定结果
| 供试菌种 | LD-P线 | EC50 | EC50标准误(×102) | EC5095％置信限 | 卡方值 |
| (y＝) | (g/L) | (Sx50) | (g/L) | x2 | |
| 小麦赤霉病菌苹果炭疽病菌番茄灰霉病菌玉米大斑病菌辣椒疫霉病菌 | 2.0804+2.9060x3.3521+1.3485x3.1681+1.9058x1.8333+2.7488x2.4214+3.2735x | 10.107816.67259.144614.19146.1335 | 3.99069.65155.13506.45506.4520 | 8.4348～12.11269.7912～28.39017.1305～11.727510.1451～19.85170.0049～0.00771 | 1.970.890.960.054.55 |
试验实施例2：孜然杀菌乳油和孜然杀菌微乳剂的田间药效试验
采用《农药田间药效试验准则》(农业部药检所生测室编，中国标准出版社出版，1993.10)中所规定的方法，对孜然杀菌乳油和孜然杀菌微乳剂的田间药效进行了试验，稀释浓度为500倍和1000倍，试验结果见表2。
表2孜然杀菌乳油和孜然杀菌微乳剂的田间药效
| 供试菌种 | 孜然杀菌乳油(防效％) | 孜然杀菌微乳剂(防效％) | ||
| 500x | 1000x | 500x | 1000x | |
| 小麦白粉病菌 | 88.5 | 81.1 | 83.4 | 74.2 |
| 苹果炭疽病菌 | 68.9 | 55.6 | 65.2 | 51.3 |
| 番茄灰霉病菌 | 80.7 | 72.1 | 79.0 | 68.5 |
| 玉米大斑病菌 | 79.3 | 60.2 | 76.5 | 58.6 |
| 辣椒疫霉病菌 | 89.5 | 75.3 | 88.6 | 76.2 |
由表2的田间药效试验表明：孜然杀菌乳油和孜然杀菌微乳剂在稀释浓度为500倍时，对供试的五种植物病原菌均有较高的防治效果。
Claims (2)
1.一种孜然杀菌剂，采用孜然的根、茎、叶、种子为原料，其特征在于，将上述原料用乙酸己酯溶剂提取，提取液经浓缩得提取物，提取物再和溶剂、农药助剂配制成孜然杀菌乳油或微乳剂；
上述杀菌剂乳油的各组份重量百分比为：
孜然提取物 50％～70％
溶剂 20％～50％
农药助剂 10％～20％
上述杀菌微乳剂的各组份重量百分比为：
孜然提取物 10％～30％
溶剂 10％～20％
水 30％～50％
农药助剂 10％～20％。
2.一种实现权利要求1所述的孜然杀菌剂的制备方法，包括杀菌剂乳油和杀菌微乳剂的制备，其特征在于：
1)杀菌剂乳油的组份重量百分比配方
孜然提取物 50％～70％
溶剂 20％～50％
农药助剂 10％～20％
2)杀菌微乳剂的配方组份重量百分比
孜然提取物 10％～30％
溶剂 10％～20％
水 30％～50％
农药助剂 10％～20％
3)其制备过程包括以下步骤：
A.将干燥的孜然根、茎、叶及种子粉碎，过40目筛；
B.用4倍于孜然粉碎物重量的乙酸己酯溶剂，在回流条件下提取，提取温度70～80℃，提取时间8h；
C.用真空浓缩的方法，将孜然提取物浓缩至与孜然原料粉碎物等重，得孜然提取物；
D.在反应釜中，按杀菌乳油配比量依次加入各成份，搅拌均匀即可得孜然杀菌乳油；
E.先将孜然提取物，农药助剂溶解于乙酸己酯溶剂中，在40℃～50℃、高速搅拌情况下将所得溶剂加入蒸馏水中，恒温搅拌1h，即得孜然杀菌微乳剂。
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| CN103004979A (zh) * | 2012-12-11 | 2013-04-03 | 甘肃农业大学 | 一种天然驱虫剂的制备方法 |
| CN103081986B (zh) * | 2013-02-28 | 2014-12-03 | 甘肃省敦煌种业股份有限公司玉门市种子公司 | 一种天然防腐剂的使用方法 |
| CN103609674A (zh) * | 2013-12-02 | 2014-03-05 | 甘肃省敦煌种业股份有限公司 | 一种预防马铃薯块茎干腐病的方法 |
| CN103651601B (zh) * | 2013-12-27 | 2015-10-28 | 成都新朝阳作物科学有限公司 | 含枯茗和牛至提取物的农药组合物及其制备方法和应用 |
| CN107646573A (zh) * | 2017-09-08 | 2018-02-02 | 广西深禾丰农业科技发展有限公司 | 一种草莓白粉病的生物防治方法 |
| CN108004022A (zh) * | 2017-12-12 | 2018-05-08 | 湖北中烟工业有限责任公司 | 用于爆珠基础油的孜然提取物的制备方法 |
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