Preparation for determination of atrazine and napropamide in water,soil and wheat | 水、土壤和小麦中阿特拉津和草萘胺残留检测的前处理方法研究

Chinese. 利用高效液相色谱检测,分别建立了水、土壤和小麦中同时检测阿特拉津和草萘胺残留量的前处理方法。对水样,用LC-18固相萃取小柱分离、净化和富集;对土壤样品,以丙酮与水（体积比3∶1）混合溶剂为提取剂振荡提取,再用LC-18固相萃取小柱分离和净化;对小麦样品,以丙酮与水（体积比3∶1）为提取剂振荡提取,石油醚萃取去杂,再用LC-18固相萃取小柱分离和净化。结果表明：高效液相色谱法同时检测阿特拉津和草萘胺的线性范围为0.05～8.0 mg・L-1,两种农药的相关系数（R2）均为1.000 0,最低检测质量浓度分别为0.02和0.03 mg・L-1。水样中阿特拉津和草萘胺加标平均回收率分别为96.13%～102.30%和94.94%～101.33%,相对标准偏差（RSD）为2.3%～2.6%和1.9%～2.9%;土壤中加标平均回收率为94.19%～103.14%和97.84%～104.51%,RSD为0.2%～3.2%和2.2%～6.2%;小麦中加标平均回收率为98.57%～107.44%和86.98%～102.91%,RSD为2.6%～3.2%和0.5%～8.1%。

English. Preparation methods for simultaneous determination of pesticides atrazine and napropamide in water,soil and wheat by high performance liquid chromatography（HPLC）were developed for the first time.Water samples were exacted,purified and collected by solid-phase extraction LC-18 column.Soil samples were extracted by acetone-water（3∶1,V/V）and purified and collected by solid-phase extraction LC-18 column.Wheat samples were extracted by acetone-water（3∶1,V/V）,and the extraction solution was extracted by petroleum ether and purified and collected by solid-phase extraction LC-18 column.The calibration curves of the methods were determined in the range of 0.05-8.0 mg・L-1 of both atrazine and napropamide,with the correlation coefficients（R2）being 1.000 0 and 1.000 0 respectively.The methods gave the limit of detection（LOD）in 0.02 and 0.03 mg・L-1 for atrazine and napropamide.The average recoveries at the three spiked levels ranged from 96.13%-102.30% and 94.94%-101.33% for water sample with the relative standard deviations（RSD）of 2.3%-2.6% and 1.9%-2.9%,94.19%-103.14% and 97.84%-104.51% for soil sample with RSD of 0.2%-3.2% and 2.2%-6.2%,and 98.57%-107.44% and 86.98%-102.91% for wheat samples with RSD of 2.6%-3.2% and 0.5%-8.1%,respectively.