摘要
针对目前国内暂无对甲氧基丙烯酸酯类杀菌剂活性基团的重要合成中间原料3-异色酮检测方法的相关研究及报道,本试验建立了一种测定3-异色酮质量分数的检测方法。采用高效液相色谱仪,以乙腈-超纯水为流动相,使用ODS-SP为填料的不锈钢色谱柱和二级阵列管检测器,在210 nm波长下对合成甲氧基丙烯酸酯类杀菌剂重要中间体3-异色酮进行分离和定量分析。当3-异色酮的质量浓度在0.5~20 mg·L^(-1)时,分析方法的线性关系良好,相关系数R^(2)为0.999,检出限为3.55×10mg·L^(-1),定量限为1.18 mg·L^(-1),土壤和水体中加标回收率均在80%以上。该检测方法分离效果好,线性关系、精密度和回收率均符合要求,可作为3-异色酮环境安全性评价时的质量分数测定方法,也可用于农药合成和生产环节的质量控制方法。
In view of the current domestic research and reports on the detection method of 3-isochromone as important intermediate for the synthesis of methoxyacrylate fungicides,a 3-isochromone detection method was established.The important intermediate3-isochromone for the synthesis of methoxyacrylate fungicides was separated and quantitatively analyzed by HPLC with acetonitrile-ultrapure water as mobile phase,ODS-SP as packing stainless steel chromatographic column and secondary array tube detector at 210 nm.When the mass concentration of 3-isochromone was 0.5~20 mg·L^(-1),the linear relationship of the method was good,the correlation coefficient R^(2)was 0.999,the detection limit was 3.55×10mg·L^(-1)and the quantitative limit was 1.18 mg·L^(-1).The recoveries in soil and water were above 80%.The method has good separation effect.The linear relationship,precision and recovery rate can meet the requirements.It can be used as a content determination method for environmental safety evaluation of 3-isochromone,and can also be used for quality control in pesticide synthesis and production.
作者
王睿
贺芳
李俊
周世阳
WANG Rui;HE Fang;LI Jun;ZHOU Shi-yang(Guizhou Testing Technology Research and Application Center,Guiyang Guizhou 550014,China;Guiyang Baiyun District Center for Disease Control and Prevention,Guiyang Guizhou 550016,China)
出处
《辽宁化工》
CAS
2022年第11期1654-1657,共4页
Liaoning Chemical Industry
基金
流域水环境质量安全的农药监测、预警、应急技术研究与示范(黔科合支撑[2021]一般464)
浙江省植物有害生物防控重点实验室--省部共建国家重点实验室培育基地(2010DS700124-KF1708)
贵州省高层次创新型人才培养计划项目资助