摇瓶法结合HPLC测定新杀菌剂唑菌酯的正辛醇-水分配系数  

Octanol/water partition coefficient determination of novel fungicide SYP-3343 by flask-shaking method using HPLC

作　　者：张海科[1] 刘秀峰[1] 范志金[1] 贾俊超[1] 钟增明[1] 徐政专[1] 刘长令[1] 

机构地区：[1]南开大学元素有机化学国家重点实验室,天津300071

出　　处：《安全与环境学报》2008年第2期5-7,共3页Journal of Safety and Environment

基　　金：国家自然科学基金项目(20672062);国家重点基础研究发展计划"973"项目(2003CB114402);天津市自然科学基金项目(07JCYBJC01200);天津市科技支撑计划国际科技合作项目(07ZCGHHZ01400)

摘　　要：为了给新型杀菌剂唑菌酯(试验代号:SYP-3343)的环境行为研究提供基本的理化参数,在建立水中微量唑菌酯高效液相色谱(HPLC)测定方法的基础上,本文采用摇瓶法测定了唑菌酯在纯水和缓冲液中的正辛醇-水分配系数。结果表明,水中的唑菌酯经二氯甲烷萃取后进行HPLC测定,HPLC测定条件为:紫外检测波长252nm,甲醇/双重蒸馏水以体积比为94/6混合作为流动相,当流速为1.0mL·min-1时,在DiamonsilC18柱(250mm×4.6mm,5μm)上有效成分可以得到很好的分离和检测。唑菌酯的保留时间约为4.2min。唑菌酯质量浓度在1.56～25μg·mL-1内相关性很好,决定系数R2为0.9999,回归方程为y=53.4960x-10.7480(x为唑菌酯浓度,y为色谱峰峰面积)。唑菌酯在0.01μg·mL-1、0.05μg·mL-1和0.2μg·mL-1质量浓度下的添加回收率分别为104.9%、106.5%和97.8%;摇瓶法测得唑菌酯在二次蒸馏水中的平均Kow为8993.59,平均lgKow为3.94±0.15;唑菌酯在pH=5.0的缓冲溶液中的平均Kow为23448.96,平均lgKow为4.37±0.12;唑菌酯在pH=9.0缓冲溶液中的平均Kow为243487.7,平均lgKow为5.36±0.26。研究结果表明,唑菌酯能很好地穿透植物叶表和真菌表皮,生物体对唑菌酯具有较强的富集作用。酸度对药剂的Kow有一定影响,但不改变药剂的高渗透性和强生物富集特性。The present article is an introduction to the author＇s method for the determination of environmental parameter Ko. of a novel fungicide SYP-3343 by way of flask shaking. SYP-3343 in water was extracted with dichloromethane, then detected by HPLC. The results showed that, under optimum condition, the retention time of SYP-3343 was about 4.2 min, the linear range was 1.56-25 μg·mL^- 1, R^2 = 0.999 9, regression equation was y = 53.4960x - 10.7480, the average fortified recoveries of SYP-3343 in water at concentration of 0.01 μg·mL^-1, 0.05 μg·mL^-1 and 0.2μg·mL^-1 were 104.9% , 106.5% and 97.8% respectively. The Kow of SYP- 3343 in double-distilled water and buffers of pH = 5.0 and pH =9.0 were 8 993.59, 23 448.96 and 243 487.7 in average respectively, the average lgKow were 3.94±0.15, 4.37±0.12 and 5.36±0.26 respectively. These results indicated that, SYP-3343 could easily penetrate the surface of plant leaf and the fungi cell wall, and the risk of biological accumulation of SYP-3343 was high, the acidity affected the lgKow of SYP-3343 in certain extents, however, because of the low hydrophihc and high lipophilic properties of this molecule, the acidity did not change its penitration and biological accumulation properties. So, it is better to take measures to aviod its harm to underground water and beneficial biologies in the fields of agricultural environment.

关 键 词：元素有机化学 唑菌酯 杀菌剂 正辛醇-水分配系数 

分 类 号：O627[理学—有机化学]