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[目的]建立一种从土壤中超声提取乙草胺和广灭灵并用高效液相色谱法测定其残留量的方法。[方法]用蒸馏水和丙酮作为提取剂超声提取土壤中的乙草胺和广灭灵,提取液经过石油醚多次萃取后,采用反相高效液相色谱法进行灵残留量测定。使用BDS Hypersil C_(18)色谱柱,以乙腈-水(体积比为70∶30)为流动相,流速为1.0 m L/min。紫外检测器检测波长为215 nm。[结果]乙草胺和广灭灵的保留时间为6.532、4.632 min,线性相关系数为0.9970和0.9983。在4个质量分数添加水平范围内,平均回收率分别为95.09%和95.50%,变异系数为3.83%和3.48%。方法检出限分别为0.163、0.0995 mg/L。[结论]该方法简单、快速、灵敏度高、准确度好,能够满足土壤中乙草胺和广灭灵残留量的检测要求。
[Objective] The research aimed to establish a method for the ultrasonic extraction of acetochlor and clomazone from soil and determination of their residues by high performance liquid chromatography. [Method] Acetochlor and clomazone in soil were extracted by ultrasonic with distilled water and acetone as extractant. The extract was extracted by petroleum ether for many times, and then the residual amount was determined by reversed-phase high performance liquid chromatography. A BDS Hypersil C_ (18) column was used with a mobile phase of acetonitrile-water (70:30 by volume) with a flow rate of 1.0 mL / min. UV detector detection wavelength of 215 nm. [Result] The retention times of acetochlor and clomazone were 6.532,4.632 min, the linear correlation coefficients were 0.9970 and 0.9983. The average recoveries were 95.09% and 95.50%, respectively, and the coefficients of variation were 3.83% and 3.48% in the range of 4 levels. The detection limits were 0.163 and 0.0995 mg / L, respectively. [Conclusion] The method was simple, rapid, sensitive and accurate, and could meet the detection requirements of acetochlor and fenugamine in soil.