【作者】 张宏浩；

【导师】 张国财；

【作者基本信息】 东北林业大学 ， 森林保护学， 2007， 硕士

【摘要】 本文首先对白屈菜粗提取物各萃取层进行赤松毛虫的生物活性测定，然后通过LC／MS／MS液／质联用分析仪对白屈菜杀虫活性成分进行测定。系统研究白屈菜全草五种提取工艺（索氏提取法、超声波提取法、微波提取法、超临界萃取法、浸渍法），通过紫外分光光度法筛选出经济、简便、高效率的白屈菜活性碱的提取方法。根据白屈菜提取物物理特性和化学特性的试验，对白屈菜农药剂型进行初探，以及田间防治时注意事项。主要研究成果如下：白屈菜活性成分初步研究表明：分别用石油醚、氯仿和正丁醇对白屈菜粗提物进行萃取，通过生物活性测定确定氯仿萃取物10倍液杀虫效果最好，校正死亡率为72.11％；其次为正丁醇萃取物1倍液，校正死亡率为56.56％；水萃取物和石油醚萃取物试虫死亡率低。LC／MS／MS液／质联用分析仪测定结果表明，白屈菜活性成分主要是异喹啉类生物碱，其中以白屈菜碱含量最为丰富，白屈菜活性碱成分中主要还有四氢黄连碱、白屈菜红碱、血根碱和黄连碱等。白屈菜提取工艺研究结果表明：提取效果依次是索氏提取法＞超声波提取法＞微波提取法＞浸渍法＞超临界萃取法，其中以70％的乙醇，90℃恒温水浴，提取时间7h的索氏提取法，提取率最高，为0.376％；其次为乙醇浓度50％，固液比0.02，超声波提取35min，提取率为0.368％。从提取率、提取时间、节约能源和实际生产考虑，得出实验室提取适合用索氏提取法，而实际生产则应采用超声波提取法。白屈菜制剂研究表明：通过白屈菜提取物的急性毒性试验，LD₅₀＞2000mg／kg，可知白屈菜提取物无严重急性中毒的危险性；白屈菜提取物易溶于水、甲醇和乙醇，很难溶于亲脂性有机溶剂；外界环境对白屈菜提取物有一定影响，加热和光照都会使白屈菜提取物稳定性变差，因此在试验过程中需注意外在条件的影响；根据白屈菜提取物物理性质和化学特性，可知白屈菜提取物适合的农药剂型为水剂、粉剂、可湿性粉剂和粒剂，使用时注意避光和高温。更多还原

【Abstract】 This thesis first has carried on the bioassay test on Dendrolimus spectabilis Butler using each extraction layer of the crude extract of Chelidonium majus L., and then used the LC/MS/MS analyzer to mensurate the insecticidal active constituent of Chelidonium majus L. We systemically studied the 5 extraction methods on Chelidonium majus L., which are Soxhlet-extraction method, Ultrasonic extraction method, Microwave extraction method, Supercritical liquid extraction method and Impregnation method. We selected the economy, simple and convenient, high-efficiency abstraction crafts of active alkaline of Chelidonium majus L. through UV-spectrophotometry. According to the test on the physical and chemical characteristics of the Chelidonium majus L. extracts, we have carried on the primary research on the pesticide agent of Chelidonium majus L. and the announcement of field control. The major research findings were as followed.The primary research on the active constituent of Chelidonium majus L. indicated that the crude extracts of were respectively extracted with the petrolum ether, Chloroform and Nbutanol and we carried on the biological activity mensuration to each extraction. The insecticidal rate of the 10 times diluents of Chloroform-extract was the best and the emendation mortality was 72.11%; the second was the once diluent of N-butanol extract and the emendation mortality was 56.56 %; the emendation mortalities of the test insects were low when water extract and petrolum ether extract were adopted. With the LC/MS/MS analyzer, the mensuration result showed that the active constituents of Chelidonium majus L. were mainly isoquinoline alkaloids, the chelidonine in the active constituents of Chelidonium majus L. was richest and there were mainly tetrahydrocoptisine, Chelerythrine, sanguinarine and hydrastis and etc. in the active alkali of Chelidonium majus L..The extraction craft of Chelidonium majus L. indicated that the extraction result was Soxhlet-extraction method＞Ultrasonic extraction method＞Microwave extraction method＞Impregnation method＞Supercritical liquid extraction method. The first was Soxhlet-extraction method, which used 70% ethanol, 90℃constant temperature water-curing and extraction time was 7h, the extraction rate was the highest 0.376%. The second was Ultrasonic extraction method, which used 50% ethanol, liquid-solid ratio 0.02 and extraction time was 35rain, the extraction rate was 0.368%. From the consideration of the extraction rate, the extraction time, the frugal energy and the mass production, we obtained that it suited with Soxhlet-extraction method when extracting tew active material in the laboratory, but the mass productions should use Ultrasonic extraction method.The primary research on the preparation of Chelidonium majus L. indicated that through the acute toxicity experiment of the Chelidonium majus L. extract (LD50＞2000mg/kg), we knew that the Chelidonium majus L. extract had no serious acute toxic risk, and it was easy to dissolve in the water, carbinol and ethanol, but was very difficult to dissolve in the lipophilic organic solvent. The external environment has certain influence on the Chelidonium majus L. extract, heating and illumination could cause the stability of the Chelidonium majus L. extract to withdraw, therefore we should pay attention to the extemal condition in the testing. According to the physical property and chemical characteristic of the Chelidonium majus L. extract, we could know that the pesticide formulations which the Chelidonium majus L. extract were suitable for were the water formulation, the soluble powder formulation and the wettable power formulation. We should avoid the light and high temperature when using it.更多还原