天然除虫菊酯化学成分制备分离及光稳定性研究  

Study on the preparation,separation of effective chemical components from natural pyrethrins and its photostability

作　　者：邓英立 丁燕[1,2] Nigel G J Richards 王寅鹏 肖伟 朱靖博 DENG Yingli;DING Yan;Nigel G J RICHARDS;WANG Yinpeng;XIAO Wei;ZHU Jingbo(School of Food and Technology,Dalian Polytechnic University,Dalian 116034,China;Institute of Plant Resource Chemistry and Application,Dalian Polytechnic University,Dalian 116034,China;School of Chemistry,Cardiff University,Cardiff CF103AT,Park Place,Wales,UK;Jiangsu Kanion Pharmaceutical Corporation Limited,Lianyungang 222001,China)

机构地区：[1]大连工业大学食品学院,大连116034 [2]大连工业大学植物资源化学与应用研究所,大连116034 [3]英国卡迪夫大学化学院,卡迪夫CF103AT [4]江苏康缘股份药业有限公司,连云港222001

出　　处：《世界农药》2020年第5期28-35,45,共9页World Pesticide

基　　金：国家自然科学基金-联合基金项目(U1603285);大连市高层次人才项目(2016RQ064)。

摘　　要：首次采用自动化真空液相色谱(AUTO-VLC)对天然除虫菊酯进行制备分离,并研究天然除虫菊酯的光稳定性及不同稳定剂对其稳定性影响。结果表明:AUTO-VLC对天然除虫菊酯有很好分离效果,实现了克级制备纯度90%以上目标物,100 g天然除虫菊酯在正己烷∶乙酸乙酯=96∶4(体积比)的分离条件下耗时16.5 h得到除虫菊酯Ⅰ(纯度93.5%)16.5 g、除虫菊酯Ⅱ(纯度>90%)13.05 g;天然除虫菊酯光降解符合一级动力学规律,光照初期除虫菊酯降解速率较高而后降解趋于平缓,太阳光下降解速率小于紫外光下且在紫外波长230 nm下更容易降解,添加稳定剂2-羟基-4-甲氧基二苯甲酮且在摩尔比1∶1时光稳定效果好。研究结果为天然除虫菊酯农药大规模生产和在农田中持久高效利用提供参考。In this paper,natural pyrethrins were separated by automatic vacuum liquid chromatography(AUTO-VLC)for the first time,and the photostability of natural pyrethrins and the effects of different stabilizers on their stability were studied.The results showed that AUTO-VLC had a good separation to natural pyrethrins and prepared the target compounds with a purity of more than 90%in gram grade.It took 16.5 h to get 16.5 g pyrethrin I(purity 93.5%)and 13.05 g pyrethrin II(purity>90%)from 100 g natural pyrethrins with the eluent of n-hexane:ethyl acetate=96:4(V∶V).The photodegradation reactions of natural pyrethrins followed the first-order kinetis.Degradation rate of pyrethrins was higher at the beginning of illumination and then lower.The degradation rate under sunlight is lower than that under ultraviolet light,and it’s easier to degrade under ultraviolet wavelength of 230 nm.When the stabilizer 2-hydroxy-4-methoxybenzophenone was used with pyrethrins and their molar ratio was 1∶1,pyrethrins had a good photostability.The results provide a reference for the large-scale production of natural pyrethrins and their sustainable and efficient utilization in farmland.

关 键 词：天然除虫菊酯 自动化真空液相色谱(AUTO-VLC) 制备分离 光稳定性 光保护剂 

分 类 号：TQ450[化学工程—农药化工]