超声萃取高效液相色谱法测定土壤中乙草胺和广灭灵残留

Simultaneous Determination of Acetochlor and Clomazone Residues in Soil by HPLC with Ultrasonic Extraction

[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。

[Aims] A method was described for determination of acetochlor and clomazone residues in soil by high-performance liquid chromatography with ultrasonic extraction. [Methods] The sample was ultrasonic extracted with extraction agent of water and acetone, and separated on the BDS Hypersil C_（18） column with a mobile phase of acetonitrile-water（70∶30, by vol） at the speed of 1.0 m L/min. The UV detector wavelength was 215 nm. [Results] The retention times for acetochlor and clomazone were 6.532 and 4.632 min, the linear correlation coefficients were 0.9970 and 0.9983, respectively. At the four spiked levels, the average recoveries for acetochlor and clomazone were 95.09 and95.50%, the relative standard deviations were 3.83 and 3.48%, the limits of detection were 0.163 and 0.0995 mg/L,respectively. [Conclusions] The method is simple, rapid, sensitive and accurate, which can meet the detection requirements for acetochlor and clomazone residues in soil.