超高效液相色谱法测定稻田水和土壤中氰氟草酯及其代谢产物

Determination of Cyhalofop-butyl and Its Pramry Metabolites Residues in Paddy Water and Paddy Soil Using Ultraperformance Liquid Chromatography

应用超高效液相色谱建立了同时测定氰氟草酯及其主要代谢物氰氟草酸在稻田水和稻田土中的残留分析方法。田水样品经二氯甲烷液液萃取,土壤采用甲醇提取,二氯甲烷萃取,外标法定量。氰氟草酯和氰氰氟草酸分别在0.001~0.5 mg/kg和0.002~0.4 mg/kg质量浓度范围内,仪器响应值与质量浓度呈良好线性关系(r>0.9999),平均回收率分别为87.66%~107.6%和73.68%~107.2%,相对标准偏差在0.71%~5.80%和0.84%~7.52%之间,氰氟草酯和氰氟草酸在田水中的最低检测浓度分别为0.001、0.002 mg/kg;氰氟草酯和氰氟草酸在土壤中的最低检测浓度分别为0.02、0.04 mg/kg。

A rapid,accurate and sensitive method was developed to determine for cyhalofop-butyl and its main metabolites（ cyhalofop-caid） residues in paddy water and paddy soil by UPLC.The water samples were cleaned up by liquid-liquid partitioning with dichloromethane.The soil samples were extracted by methanol and detected by UPLC.The linearity was satisfied（ r 0.9999） in the concentration range of 0.001 - 0.5 mg/kg with correlation coefficients.The average recoveries varied from 73.68% to 107.6% and relative standard deviation varied from 0.71% to 7.52% when cyhalofop-butyl and cyhalofop-caid were fortified in various matrixes.The limit of detection（ LOD） of cyhalofop-butyl calculated as a sample concentration was 0.001 mg/kg-（-1） and 0.02 mg/kg-（-1） for paddy water and for soil.The limit of detection（ LOD） of cyhalofop-caid calculated as a sample concentration was 0.002 mg/kg-（-1） and 0.04 mg/kg-（-1） for paddy water and for soil.