CN112493240A - 一种用于西红柿青枯病的防治剂及其制备方法 - Google Patents
一种用于西红柿青枯病的防治剂及其制备方法 Download PDFInfo
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- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/14—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
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- A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
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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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- A01N47/42—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 the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides containing —N=CX2 groups, e.g. isothiourea
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- C07D—HETEROCYCLIC COMPOUNDS
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Abstract
本发明涉及提供了一种防治西红柿青枯病的药物组合物，本发明提供了一种防治西红柿青枯病的药物组合物，包括如下质量百分比的原料：1‑5％复合抗菌剂，溶剂60‑90％，助剂5‑15％。所述复合抗菌剂的活性成分包括白杨素和新植霉素，所述白杨素和新植霉素的重量比为1:10‑10:1。经实验证实，白杨素对新植霉素抑制青枯菌的效果具有明显的增效作用，其中，白杨素和新植霉素的重量比为1:1时效果最佳。本发明复合抗菌剂能有效降低青枯病的发生率，降低成本，提高用药安全性，在农业抗菌剂领域具有广阔的应用前景。
Description
技术领域
本发明涉及植物保护技术的生物防治领域，尤其涉及西红柿青枯病的防治剂。
背景技术
西红柿青枯病又名西红柿细菌性枯萎。青枯病的特征是发病时间短、蔓延速度非常快，如果严重会导致西红柿植株的成片死亡，致使蔬菜种植户的经济效益受到极大的影响。植株感病后，植株地上部中午时最初呈轻度萎蔫状，黄昏、夜间至早晨仍能恢复。伴随病势继续扩展，全株叶片急剧失水萎蔫，枯萎的叶片仍保持绿色。地上部出现萎蔫后，拔起植株，可见主根尖端变褐色软腐状；剖视茎部维管束为黄褐色至黑褐色。在土壤潮湿的情况下，用手挤压病株，在病部即可流出污白色的细菌益脓。青枯病主要危害西红柿、茄子、辣椒、土豆、生姜等农作物。当没有宿主时，病原体可在土壤中存活长达14个月并能够在土壤中越冬，因此低温很难根除青枯假单胞菌，这种病菌主要通过雨水、灌溉水和农具传播，患病的马铃薯块和肥料也能携带病原体。因此一旦有病残体残留，青枯病原体就极易从根或茎基部伤口侵入，并在植物的血管组织中扩散生长，导致导管堵塞和西红柿植株细胞中毒。
紫果西番莲PassifloraedulisSims是西番莲科西番莲属植物，是我国栽种面积最广泛的品种之一，目前在我国台湾、福建、广东、广西和云南等地均有栽培。其果实因具有怡人的香味与丰富的营养而深受人们喜爱。在北美及欧洲，多种西番莲叶提取物已作药用，具有抗氧化、抗焦虑、镇静、抗菌消炎、利尿、滋补等作用，在治疗酒精、尼古丁、吗啡以及大麻酚的药物成瘾性上也有很好的疗效。西番莲叶提取物在一些国家已被批准临床应用，并被正式列入了美国药典、英国药典、巴西药典、瑞典药典以及其他一些国家的药典。白杨素是西番莲的主要成分之一，有关白杨素的研究主要集中在其对抗焦虑、抗癌、降血脂等的贡献，利用白杨素作为防治作物青枯病增效剂的研究还未见报道。
发明内容
本发明的目的在于提供一种防治西红柿青枯病的药物组合物，解决了现有的西红柿青枯病农药种类缺乏、防治效果不够理想的问题。
为解决上述技术问题，本发明是通过以下技术方案实现的：
本发明的目的在于提供一种防治西红柿青枯病的复合抗菌剂，所述复合抗菌剂的活性成分包括白杨素和新植霉素，所述白杨素和新植霉素的重量比为1:10-10:1；优选的，所述白杨素和新植霉素的重量比为1:3-3:1；更优选的，所述白杨素和新植霉素的重量比为1：1。
本发明的优选技术方案中，所述白杨素的制备方法为：
(1)制备白杨素提取浸膏：精密称取经石油醚冷浸脱脂后的紫果西番莲叶，加入2-5倍量的30-50％乙醇，浸泡30min，加热回流提取1-4次，每次2.5h，过滤，合并滤液，减压回收溶剂，加入2-6倍量石油醚于室温下静置2h，出现絮状沉淀，加入活性炭，搅拌吸附，减压浓缩成浸膏；
(2)白杨素化合物的纯化：以适量乙醚溶解上述白杨素提取浸膏，用硅胶(300-400目)分离柱层析，以石油醚(60-90℃)-乙酸乙酯(5∶1→1∶1)为洗脱剂进行梯度洗脱，合并石油醚-乙酸乙酯(1∶1)的组分，用硅胶(300-400目)柱层析，以氯仿-甲醇(5∶3)为洗脱剂进行洗脱，将所得组分继续采用硅胶(300-400目)柱层析，以氯仿-甲醇(20∶1)为洗脱剂洗脱，最后将所得组分采用硅胶(300-400目)柱层析，以石油醚-丙酮(1:0→0:1)为洗脱剂进行梯度洗脱，收集石油醚-乙酸乙酯(0∶1)的组分，以乙醚为溶剂进行重结晶，即得。
本发明的优选技术方案中，所述白杨素化合物的纯度在85％以上。
本发明另一目的在于提供一种防治西红柿青枯病的药物组合物，包括如下质量百分比的原料：1-5％复合抗菌剂，溶剂60-90％，助剂5-15％
本发明的优选技术方案中，所述溶剂选自水、乙醇、丙酮、乙二醇、丙三醇、异丙醇、DMSO中的任一种或其组合。
本发明的优选技术方案中，所述助剂选自分散剂、崩解剂、增稠剂、乳化剂、防腐剂、润湿剂中的一种或几种组合。
本发明的优选技术方案中，所述药物组合物的制备方法为：向溶剂中加入白杨素和新植霉素，加入助剂，充分搅拌，即得。
本发明另一目的在于提供白杨素用于提高新植霉素对茄科植物的青枯病防治效果中的应用，优选的，所述茄科植物为西红柿。
本发明另一目的在于提供复合抗菌剂防治茄科植物的青枯病中的应用，优选的，所述茄科植物为西红柿。
本发明取得了下述有益效果：
白杨素对新植霉素抑制青枯菌的效果具有明显的增效作用；白杨素和新植霉素的重量比为1:1时效果最佳。
本发明复合抗菌剂能有效降低青枯病的发生率，降低成本，提高用药安全性，在农业抗菌剂领域具有广阔的应用前景。
具体实施方式
实施例1白杨素化合物的制备
(1)白杨素提取浸膏的制备：精密称取经石油醚冷浸脱脂后的紫果西番莲叶200g，加入3倍量45％乙醇，浸泡30min，于50℃加热回流提取2次，每次2.5h，过滤，合并滤液，减压回收溶剂，加入3倍量石油醚于室温下静置2h，出现絮状沉淀，加入200目活性炭，搅拌吸附30s，过滤，40℃减压浓缩成浸膏；
(2)白杨素的纯化：以适量乙醚溶解所述白杨素提取浸膏，用硅胶(300-400目)分离柱层析，以石油醚(60-90℃)-乙酸乙酯(5∶1→1∶1)为洗脱剂进行梯度洗脱，合并石油醚-乙酸乙酯(1∶1)的组分，用硅胶(300-400目)柱层析，以氯仿-甲醇(5∶3)为洗脱剂进行洗脱，将所得组分继续采用硅胶(300-400目)柱层析，以氯仿-甲醇(20∶1)为洗脱剂洗脱，最后将所得组分采用硅胶(300-400目)柱层析，以石油醚-丙酮(1:0→0:1)为洗脱剂进行梯度洗脱，收集石油醚-丙酮(0∶1)的组分，以乙醚为溶剂进行重结晶，即得白杨素化合物。
实施例2白杨素含量检测
将实施例1所得白杨素化合物用70％的乙腈稀释，采用液相色谱方法检测白杨素含量。仪器条件为：色谱柱：ODS-C18色谱柱(250mm×4.6mm，5μm)；流动相：乙腈-0.2％磷酸(20:80)；流速：1.0mL·min-1；进样量：10μL；柱温：35℃；检测波长：220nm。经检测，上述白杨素化合的纯度为88.93％。
实施例3本发明复合抗菌剂的制备
按表1配方，将实施例2获得的白杨素、新植霉素1在容器中混匀，必要时通过高速搅拌获得均匀稳定的配方1-7。
表1配方1-7配方
| 编号 | 白杨素(mg) | 新植霉素(mg) |
| 配方1 | 40 | 0 |
| 配方2 | 35 | 5 |
| 配方3 | 30 | 10 |
| 配方4 | 20 | 20 |
| 配方5 | 10 | 30 |
| 配方6 | 5 | 35 |
| 配方7 | 0 | 40 |
注1：新植霉素购自上海国际农化责任有限公司。
实施例4本发明复合抗菌剂对青枯病菌的体外抑制试验适量丙酮溶解实施例3的配方1-7，以去离子水稀释至40mg/ml。
供试菌株为T1130-青枯菌(生化型I型)，-80℃冷冻保存。试验前于NA(蛋白胨10g，葡萄糖10g，牛肉膏3g，水1000mL，pH7.0)培养基上活化，30℃下培养48-72h后，配制浓度为1.0×106CFU/ml的菌液待用。
用移液枪分别吸取0.1ml相应的菌悬液于琼脂平板上，用灭菌涂布棒涂布均匀，在涂有菌悬液的培养皿表面垂直放上3个牛津杯，杯子中分别加入200μl待检样品、200μl阴性对照和200μl阳性对照。平板于超净工作台内放置4h确保试剂充分扩散到琼脂中，并置于37℃培养箱下培养24h，观察结果，并用十字交叉法测定抑菌圈直径，重复4次测量，取平均值。白杨素对青枯病菌的抑菌效果，如表1所示。
表1白杨素对青枯病菌的抑抑菌效果
| 待测品 | 抑菌圈直径mm |
| 配方1 | 13.23±0.63 |
| 配方2 | 15.42±0.72 |
| 配方3 | 26.78±1.23 |
| 配方4 | 28.98±0.53 |
| 配方5 | 23.45±0.94 |
| 配方6 | 16.11±0.09 |
| 配方7 | 19.42±0.65 |
表1结果表明：白杨素联合新植霉素对T1130-青枯菌的抑制作用较新植霉素单独用药更加优异，说明白杨素联合新植霉素具有明显的增效作用。白杨素和新植霉素的重量比为1:3-3:1时效果较好，白杨素和新植霉素的重量比为1:1时效果最佳，最大抑菌圈直径达28.98mm。本发明复合抗菌剂对T1130-青枯菌具有明显的拮抗活性。
实施例5本发明复合抗菌剂对青枯病的盆栽防治效果
西红柿种子经75％乙醇灭菌后催芽，在花盆中的灭菌土中播种，按常规管理。当西红柿苗培养至2-3片真叶时，用下述浸根法和浇灌法进行盆栽试验，每个处理4个重复，每盆5棵植物。
浸根法：适量丙酮溶解实施例3的配方1-7，以去离子水稀释至浓度为40mg/ml，将西红柿苗根部浸入上述溶液；
浇灌法：适量丙酮溶解实施例3的配方1-7，以去离子水稀释至浓度为40mg/ml，对西红柿苗进行灌根(50ml/株)。
处理48h后，用伤根灌菌法接种T1130-青枯菌，菌悬液浓度为3×108cfu/mL，接种量为5ml/株。接种后室温升至30℃以利发病。接种后21d记录发病情况，分析检测白杨素对西红柿青枯病菌的抑制作用。
西红柿青枯病病情调查分级标准如下：0级：无症状；1级：1片叶萎蔫；2级：2-3片叶萎蔫；3级：4片叶以上萎蔫；4级：整株萎蔫或死亡。
病情指数＝Σ(各级发病指数×级别)/(调查总株数×最高级别)×100％
防治效果(％)＝(对照区病情指数-处理区病情指数)/对照区病情指数×100％。
结果如下：
表2白杨素对青枯病的盆栽防治效果
表2结果表明，本发明复合抗菌剂浸根和浇灌处理对西红柿青枯病的发生具有良好的抑制作用，白杨素和新植霉素的重量比为1:3-3:1时效果较好，白杨素和新植霉素的重量比为1:1时效果最佳，能较好的防控西红柿青枯病的发生和发展。
实施例6本发明制剂的制备
称取1g白杨素和2g新植霉素，加入50ml丙三醇，20ml异丙醇以充分溶解，加入十二烷基苯磺酸钠2g，苯乙烯基苯酚聚氧乙烯醚5g，充分搅拌，即得。
以上实施例描述了本发明的一些示例性实施例，但是对本领域的技术人员来说，在不脱离本发明的原理和精神的情况下，还可以对这些示例性实施例做出若干修改，本发明的范围以权利要求所限定的保护范围为准。
Claims (10)
1.一种防治西红柿青枯病的复合抗菌剂，其特征在于，所述复合抗菌剂的活性成分包括白杨素和新植霉素，所述白杨素和新植霉素的重量比为1:10-10:1；优选的，所述白杨素和新植霉素的重量比为1:3-3:1；更优选的，所述白杨素和新植霉素的重量比为1：1。
2.根据权利要求1所述的复合抗菌剂，所述白杨素的制备方法包括如下步骤：(1)白杨素提取浸膏的制备：精密称取经石油醚冷浸脱脂后的紫果西番莲叶，加入2-5倍量的30-50％乙醇，浸泡30min，加热回流提取1-4次，每次2.5h，过滤，合并滤液，减压回收溶剂，加入2-6倍量石油醚于室温下静置2h，出现絮状沉淀，加入活性炭，搅拌吸附，减压浓缩成白杨素浸膏；
(2)白杨素化合物的纯化：以适量乙醚溶解所述白杨素浸膏，用硅胶(300-400目)分离柱层析，以石油醚(60-90℃)-乙酸乙酯(5∶1→1∶1)为洗脱剂进行梯度洗脱，合并石油醚-乙酸乙酯(1∶1)的组分，用硅胶(300-400目)柱层析，以氯仿-甲醇(5∶3)为洗脱剂进行洗脱，将所得组分继续采用硅胶(300-400目)柱层析，以氯仿-甲醇(20∶1)为洗脱剂洗脱，最后将所得组分采用硅胶(300-400目)柱层析，以石油醚-丙酮(1:0→0:1)为洗脱剂进行梯度洗脱，收集石油醚-乙酸乙酯(0∶1)的组分，以乙醚为溶剂进行重结晶，即得白杨素化合物。
3.根据权利要求1-2任一项所述的复合抗菌剂，所述白杨素化合物的纯度在85％以上。
4.一种防治西红柿青枯病的药物组合物，其特征在于，包括如下质量百分比的原料：1-5％复合抗菌剂，溶剂60-90％，助剂5-15％。
5.根据权利要求4所述的药物组合物，所述溶剂选自水、乙醇、丙酮、乙二醇、丙三醇、异丙醇、DMSO中的任一种或其组合。
6.根据权利要求4-5任一项所述的药物组合物，所述助剂选自分散剂、崩解剂、增稠剂、乳化剂、防腐剂、润湿剂中的一种或几种组合。
7.根据权利要求4-6任一项所述药物组合物的制备方法，其特征在于，包括如下步骤：称取白杨素和新植霉素，加入溶剂以充分溶解，加入助剂，充分搅拌，即得。
8.根据权利要求7所述的制备方法，包括如下步骤：称取1g白杨素和2g新植霉素，加入50ml丙三醇，20ml异丙醇以充分溶解，加入十二烷基苯磺酸钠2g，苯乙烯基苯酚聚氧乙烯醚5g，充分搅拌，即得。
9.根据权利要求1-3任一项所述的复合抗菌剂防治茄科植物的青枯病中的应用，优选的，所述茄科植物为西红柿。
10.白杨素用于提高新植霉素对茄科植物的青枯病防治效果中的应用，优选的，所述茄科植物为西红柿。
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