17%烯草酮·乙羧氟草醚乳油高效液相色谱分析

Analysis of clethodim·benzofluorfen 17%EC by HPLC

建立一种对17%烯草酮·乙羧氟草醚乳油中的有效成分同时进行分离和测定的正、反相高效液相色谱方法,并考察正、反相高效液相色谱法对烯草酮与乙羧氟草醚的检测差异。正相方法采用Syncronis Silica不锈钢柱和紫外检测器,在波长230 nm条件下,以二氯甲烷-正己烷-冰乙酸(28∶70∶2,体积比)为流动相,对试样中烯草酮和乙羧氟草醚的含量进行分离和定量分析;反相方法采用安捷伦SB-C_(18)不锈钢柱和紫外检测器,在波长230 nm条件下,以乙腈-1%冰乙酸水溶液(80∶20,体积比)为流动相,对试样中烯草酮和乙羧氟草醚的含量进行分离和定量分析。正相方法中烯草酮和乙羧氟草醚的标准偏差分别为0.02和0.04,相对标准偏差分别为0.18%和0.76%,平均回收率分别为99.64%和99.24%,线性相关系数均为0.9995;反相方法中烯草酮和乙羧氟草醚的标准偏差分别为0.03和0.01,相对标准偏差分别为0.29%和0.14%,平均回收率分别为98.36%和99.49%,线性相关系数分别为0.9995和0.9993。2种方法均重现性好、准确度高、分离效果好,均适用于该混配制剂中烯草酮和乙羧氟草醚的定量分析和质量控制。

Normal phase method and reversed phase method for separation and quantitative analysis of simultaneous determination in clethodim·benzofluorfen 17%EC was established by HPLC.At the same time,the detection differences between clethodim and benzofluorfen by normal phase method and reversed phase HPLC method.Normal phase HPLC method using Syncronis Silica-C18 column as stainless steel pillar stuffed,UV wavelength 230 nm,the mixture solution of dichloromethane-n-hexane-glacial acetic acid(28:70:2,by vol)as the mobile phase by HPLC.Reversed phase HPLC method using Agilent SB-C_(18) column as stainless steel pillar stuffed,UV wavelength 230 nm,the mixture solution of acetonitrile-1%acetic acid(AC)aqueous solution(80:20,by vol)as the mobile phase by HPLC.The results showed that,under the normal phase condtion,the standard deviations of clethodim and benzofluorfen were 0.02 and 0.04,the relative standard deviations were 0.18%and 0.76%,the average recoveries were 99.64%and 99.24%,and the linear correlation coefficients between the concentrations of clethodim or benzofluorfen and their responding values were all 0.9995,respectively.Under the reversed phase condtion,the standard deviations of clethodim and benzofluorfen were 0.03 and0.01,the relative standard deviations were 0.29%and 0.14%,the average recoveries were 98.36%and 99.49%,and the linear correlation coefficients were 0.9995 and 0.9993,respectively.The methods have several advantages such as good reproducibility,high accuracy and separation,and it is suitable for quantitative analysis and quality control of clethodim and benzofluorfen in the mixture formulation.