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采用氢氧化钠-甲醇溶液提取,二氯甲烷萃取,定量甲醇、浓H2SO4条件下酯化,气相色谱法测定小麦及土壤中的氯氟吡氧乙酸。氯氟吡氧乙酸质量浓度在0.01~1.0 mg.L-1之间线性关系良好。在添加浓度0.01~0.8 mg.kg-1下,植株、土壤和籽粒中氯氟吡氧乙酸的平均回收率分别为72.3%~86.7%、83.6%~95.8%和77.7%~87.3%,变异系数分别为3.02%~8.59%、2.87%~8.46%和2.75%~7.61%。氯氟吡氧乙酸的最小检测量为1.0×10-11g,在植株、土壤和籽粒中最低检出浓度均为0.01 mg.kg-1。该方法的准确性、精确性和灵敏度均满足农药残留分析的要求。
The crude extracts were extracted with sodium hydroxide-methanol solution, extracted with methylene chloride, and quantified by methanol. Esterification was carried out under concentrated H2SO4 and the flurbiprofen in wheat and soil was determined by gas chromatography. Fluroxypyr concentration of 0.01 ~ 1.0 mg.L-1 between the good linear relationship. The average recoveries of flurbiprofen in plant, soil and grain were 72.3% -86.7%, 83.6% -95.8% and 77.7% -87.3% at the concentration of 0.01-0.8 mg.kg-1, respectively. The coefficient of variation Respectively 3.02% ~ 8.59%, 2.87% ~ 8.46% and 2.75% ~ 7.61%. The minimum detectable amount of flurbiprofen was 1.0 × 10-11 g, and the lowest detectable concentrations in plant, soil and grain were 0.01 mg.kg-1. The accuracy, accuracy and sensitivity of this method all meet the requirements of pesticide residue analysis.