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建立了二氯甲烷萃取浓缩,反相高效液相色谱测定水样中甲基磺草酮农药含量的分析方法。调节水样pH值为4.0后,以二氯甲烷为萃取剂,25℃下重复萃取两次,萃取时间为15min,旋转蒸发仪浓缩近干,乙腈定容。以SPHERI-5RP-18(5Lm)为色谱柱,乙腈-磷酸缓冲溶液(pH值4.0)为流动相,紫外检测波长为220nm。结果表明,在选定的萃取和色谱条件下,甲基磺草酮测定的线性范围为0.5—100.0mg/L,线性相关系数r为0.9996,标准偏差(SD)为0.46,变异系数(CV)为0.47%,平均加标回收率88.9%,检出限为0.03mg/L。此方法可用于实际水样中甲基磺草酮农药含量的测定。
A method for the determination of mesotrione pesticide in water samples by dichloromethane extraction and concentration and reversed-phase high performance liquid chromatography was established. After the water sample was adjusted to pH 4.0, dichloromethane was used as extractant and extracted twice at 25 ℃. The extraction time was 15 min. The residue was concentrated to near dryness on a rotary evaporator and the volume of acetonitrile was fixed. The mobile phase was acetonitrile-phosphoric acid buffer solution (pH 4.0) with SPHERI-5RP-18 (5Lm) as the mobile phase. The UV detection wavelength was 220 nm. The results showed that the linear range of determination of mesotrione was 0.5-100.0mg / L under the conditions of selected extraction and chromatographic conditions, the linear correlation coefficient was 0.9996, the standard deviation (SD) was 0.46, the coefficient of variation (CV) 0.47%, the average recovery of 88.9%, the detection limit of 0.03mg / L. This method can be used for the determination of mesotrione pesticide content in actual water samples.