【摘要】 [目的]建立同时测定大豆中苯达松、三氟羧草醚、氟磺胺草醚、苯草醚、甲羧除草醚、精恶唑禾草灵、除草醚、乙羧氟草醚、乙氧氟草醚9种二苯醚类除草剂多残留量的高效液相色谱分析方法。[方法]将样品中的二苯醚类除草剂用乙腈提取、凝胶色谱和Florisil固相萃取小柱净化后,经C8色谱柱分离,采用二极管阵列检测器检测。[结果]对样品的提取、净化及液相色谱的分离条件进行了优化。待测9种二苯醚类除草剂在0.10～10.0mg/L质量浓度范围内呈良好的线性关系,相关系数r=0.9971～0.9998,方法的精密度RSD为1.49%～4.65%,在0.05～0.5mg/kg的添加水平范围内,加标回收率为75.4%～101.9%,方法的检出限(S/N=3)为6.9～36μg/kg。同时对待测除草剂的液相色谱-质谱确证实验进行了研究。[结论]所建立的方法简便、快速,适用于大豆中9种二苯醚类除草剂残留量的同时测定。更多还原

【Abstract】 [Objective]To establish a rapid analytical method for the determination of nine biphenyl ether herbicides(bentazone,acifluorfen,fomesafen,aclonifen,bifenox,fenoxaprop-p-ethyl,nitrofen,fluoroglycofen-ethyl,oxyfluorfen)in soybean by high performance liquid chromatography(HPLC)with diode array detector detection.[Methods]The residues of nine herbicides were extracted with acetone from soybeans and the extract was cleaned up with a gel permeation chromatography and Florisil solid phase extraction column.The analytes were separated by using Carbamate Analysis C8 column and acetonitrile-water(containing 0.05% triethylamine,v/v)as mobile phase with gradient elution and detected by a diode array detector set.[Results]There was good linear correlation between the concentrations and peak of analytes in the range was 0.05mg/kg-0.5mg/kg with the correlation coefficient of 0.997 1-0.999 8.The recoveries were 75.4%-101.9% with relative standard deviations(n = 5)of 1.49%-4.65%.The limits of detection(S/N=3)was 6.90 μg/kg-36.0 μg/kg.At the same time,the analytes were qualitatively corroborated by HPLC-MS.[Conclusion]The results indicate that the proposed method is suitable to the determination of biphenyl ether herbicides in soybean.更多还原