CN110563744B - 一种防治园林内夜蛾的化合物及应用 - Google Patents
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Abstract
本发明属于园林虫害防治技术领域，涉及到一种防治园林内夜蛾的化合物及应用。将新鲜的黄花蒿嫩叶加水提取，大孔树脂分离，半制备高效液相追踪并制备，重结晶即得该化合物，命名为黄花蒿素酸，为新化合物。本发明所述防治园林内夜蛾的化合物，来自于天然药物黄花蒿，黄花蒿作为药物，其提取物曾被多次用于临床，对人体无明显副作用，安全性好，活性实验也表明黄花蒿素酸对夜蛾具有良好的灭杀作用，具有广阔的应用前景。
Description
技术领域
本发明属于园林虫害防治技术领域，具体涉及到一种防治园林内夜蛾的化合物及应用。
背景技术
夜蛾指的是夜蛾科的一类昆虫，多为植食性害虫，少数种类捕食其他昆虫。某些种类成虫喙很强，能刺穿果皮吸食果汁，还有少数种类能吮吸人、畜的分泌物。夜蛾科许多种类在大量发生时，会给树木及农作物造成大害。例如，小造桥夜蛾的幼虫就会为害悬铃木、柑橘、木槿、木芙蓉、海桐、芒果、扶桑、锦葵和大红花等叶片，把叶片食光，只留下叶脉，影响花木观赏效果。还有卷叶蛾，还为害苹果、沙果、桃、梨、李等果树，其幼虫幼虫为害叶片时，吐丝将2～3张叶片缀连在一起，在其中取食，将叶片吃成网状或缺刻。
对于园林病虫害的防治，主要的夜蛾方法有：春季或初冬刮除老翘皮、剪锯口周围死皮组织，伤口周围死皮组织，消灭越冬幼虫；果树树芽萌动前，用敌敌畏稀释50倍液或(毒斯脾30倍液)+助剂涂抹剪锯口、伤口、老翘皮，可杀死大量越冬幼虫。但是刮除树皮既麻烦且对树木有损害，而用于杀灭夜蛾的敌敌畏则毒性太大，对操作人员及园林的观赏人员都有危害。后续虽也有较多的杀灭夜蛾药物开发出来，但对人体毒性小且却能高效杀灭夜蛾的药物却较少。
发明内容
为解决上述技术问题，本发明发现了一种防治园林内夜蛾的化合物。该化合物来自于天然产物，对夜蛾具有很好的灭杀作用。
本发明所述的一种防治园林内夜蛾的化合物，命名为黄花蒿素酸，黄花蒿素酸具体结构如下所示：
所述黄花蒿素酸的制备方法为：将新鲜的黄花蒿嫩叶加入8-12倍量的水，匀浆后再过滤得到滤液，滤液上大孔树脂柱，大孔树脂填料重量为滤液干膏重的30倍，先用70％的乙醇洗脱10以上倍体积，紧接着再用75-80％的乙醇洗5倍体积，合并75-80％乙醇洗脱液，去除溶剂，得黄花蒿制备物；再取黄花蒿制备物，30倍量甲醇溶解，0.22um滤膜过滤，取滤液，进半制备高效液相，检测波长292nm并以质谱追踪，梯度洗脱，流速1.0ml/min，洗脱时间0.5h，流动相变化为从甲醇比水3:7到甲醇比水9:1，收集12-15min时间段中含分子量信号为326.1366的洗脱液，浓缩，重结晶即得。
黄花蒿素酸的应用，用于园林内夜蛾的防治。尤其是银纹夜蛾、斜纹夜蛾、小造桥夜蛾及苹小卷叶蛾。
本发明所述防治园林内夜蛾的化合物黄花蒿素酸为新化合物，来自于天然药物黄花蒿，黄花蒿作为药物，其提取物曾被多次用于临床，对人体无明显副作用，安全性好，活性实验也表明黄花蒿素酸对夜蛾具有良好的灭杀作用，具有广阔的应用前景。
附图说明
图1：本发明所涉及的新化合物黄花蒿素酸的结构式。
具体实施方式
下面结合具体实施例对本发明所述防治园林内夜蛾的化合物作进一步说明，但是本发明的保护范围并不限于此。
实施例1
将新鲜的黄花蒿嫩叶加入10倍量的水，匀浆后再过滤得到滤液，滤液上D101大孔树脂柱，大孔树脂填料重量为滤液干膏重的30倍，先用70％的乙醇洗脱10倍柱体积，紧接着再用75％的乙醇洗5倍柱体积，合并75％乙醇洗脱液，去除溶剂，得黄花蒿制备物。取黄花蒿制备物，30倍量甲醇溶解，0.22um滤膜过滤，取滤液，进半制备高效液相，检测波长292nm并以质谱追踪，梯度洗脱，流速3.0ml/min，洗脱时间0.5h，流动相变化为从甲醇比水3:7到甲醇比水9:1，收集12-15min时间段中含分子量信号为326.1366的洗脱液，浓缩，重结晶即得。新化合物黄花蒿素酸结构鉴定：无色晶体，HRMS：m/z＝326.1362([M-H]-，calc.forC16H22O6325.1284)；1HNMR(300MHz，CDCl3)δppm：1.41(1H，J1-10α＝6.8，J1-10β＝11.2，C1-H)，1.46(1H，J2-14＝6.1Hz，C2-H)，1.79，1.09(1H，C3-H)，1.86，1.08(1H，C4-H)，1.79(1H，J5-11＝5.0，C5-H)，5.87(C7-H)，2.01，1.55(2H，J9α-9β＝14.6，J9α-10β＝3.8，J9α-10β＝13.4，C9-H)，2.31(H，J9α-10β＝3.8，J9α-10β＝13.4，C10-H)，3.40(1H，J11-13＝7.1，C11-H)，1.22(3H，C13-H)，1.01(3H，C15-H)，1.46(3H，C16-H)，11.23(1H，OH)。13C-NMR(300MHz，CDCl3)δppm：51.24，(C1)，37.87(C2)，34.08(C3)，23.11(C4)，46.04(C5)，80.03(C6)，91.44(C7)，104.92(C8)，22.84(C9)，53.21(C10)，32.84(C11)，172.23(C12)，12.65(C13)，182.12(C14)，19.98(C15)，26.02(C16)。
活性测试
将黄花蒿素酸用50％的乙醇稀释成质量浓度分别为2、6、18、54mg/ml的溶液，将银纹夜蛾、斜纹夜蛾、小造桥夜蛾及苹小卷叶蛾的3龄幼虫浸于不同质量浓度的黄花蒿素酸溶液中3s，置于吸水纸上晾干，置于装有人工饲料的48孔培养板中，每板处理不同夜蛾各10只，以50％的乙醇作为对照设两孔，重复3次，分别统计处理后第3，7天的夜蛾死亡情况，计算平均死亡率。轻触虫体，不动或不能正常爬动者计为死亡。结果见表1。
表1：黄花蒿素酸对夜蛾杀灭效果(平均死亡率，％)
Claims (3)
1.一种防治园林内夜蛾的化合物，其特征在于，其命名为黄花蒿素酸，所述黄花蒿素酸具体结构如下所示：
所述化合物的制备方法为：将新鲜的黄花蒿嫩叶加入8-12倍量的水，匀浆后再过滤得到滤液，滤液上大孔树脂柱，大孔树脂填料重量为滤液干膏重的30倍，先用70％的乙醇洗脱10以上倍体积，紧接着再用75-80％的乙醇洗5倍体积，合并75-80％乙醇洗脱液，去除溶剂，得黄花蒿制备物；再取黄花蒿制备物，30倍量甲醇溶解，0.22um滤膜过滤，取滤液，进半制备高效液相，检测波长292nm并以质谱追踪，梯度洗脱，流速1.0ml/min，洗脱时间0.5h，流动相变化为从甲醇比水3:7到甲醇比水9:1，收集12-15min时间段中含分子量信号为326.1366的洗脱液，浓缩，重结晶即得。
2.根据权利要求1所述的化合物的应用，其特征在于，其用于园林内夜蛾的防治。
3.根据权利要求2所述的应用，其特征在于，夜蛾为银纹夜蛾、斜纹夜蛾、小造桥夜蛾及苹小卷叶蛾。
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