Gas-Liquid Chromatographic Determination of Haloxyfop-R and lts Methyl Ester Residues in Soils and Soybeans

토양과 대두중 Haloxyfop-R 및 Haloxyfop-R-methyl의 기체크로마토그래피를 이용한 잔류분석

  • Lee, Young-Deuk (Dept. of Argricultural Chemistry,College of Natural Resource,Taegu University)
  • Published : 1997.12.30

Abstract

An analytical method was developed to determine residues of haloxyfop-R and its methyl ester in soils and soybeans using gas-liquid chromatography (GLC) with electron capture detector (ECD). Soil or soybean sample was acidified and extracted with acetone. The extract was then subjected to ion-associated partition to individually separate haloxyfop-R and the neutral methyl ester. One phase containing haloxyfop-R was methylated with $BF_3$/methanol, partitioned to n-hexane and analyzed by GLC/ECD. The other phase containing the methyl ester was further purified by Florisil column chromatography prior to GLC determination. No cross contamination was found between two phases containing each of the acid and methyl ester, thus two compounds can be separately determined as the identical haloxyfop-R-methyl. Overall recoveries of haloxyfop-R from fortified samples averaged 88.2${\pm}$3.9% (n=12) and 88.3${\pm}$4.0% (n=6) for soils and soybeans respectively, and those of haloxyfop-R-methyl showed mean values of 89.2${\pm}$4.0% (n=12) and 85.6${\pm}$5.6% (n=6). Detection limits of both haloxyfop-R and its methyl esterwere 0.005㎎/㎏ and 0.01㎎/㎏ for soil and soybean samples respectively.

Keywords

haloxyfop-R;haloxyfop-R-methyl;residue analysis;soil;soybean;GLC