高效液相色谱法检测吡唑醚菌酯在烟叶和土壤中的残留及消解动态  

Residue and dissipation of pyraclostrobin by high performance liquid chromatography in tobacco and soil

作　　者：闫晓阳[1,2] 徐金丽[1] 徐光军[1] 杨立强[1,2] 宋超[1,2] 李义强[1] 王秀国[1] 

机构地区：[1]中国农业科学院烟草研究所/国家烟草专卖局病虫害监控与综合治理重点实验室,山东青岛266101 [2]中国农业科学院研究生院,北京100081

出　　处：《农药学学报》2013年第5期528-533,共6页Chinese Journal of Pesticide Science

基　　金：国家自然科学基金项目(41201291);国家烟草专卖局重点项目(TS-06-20110039;110200902073)

摘　　要：研究建立了吡唑醚菌酯在烟叶和土壤中残留及消解动态的高效液相色谱分析方法。样品用乙腈提取，经固相萃取柱SPE-C18和SPE-PSA净化，高效液相色谱-二极管阵列检测器（HPLC-DAD）检测，外标法定量。结果表明：在0．0～2mg!kg添加水平下，吡唑醚菌酯在烟叶和土壤中的平均回收率分别为97．5％～101．9％和93．4％～101．2％，相对标准偏差（RSD）分别为4．8％～6．8％和1．5％～10．5％。吡唑醚菌酯在烟叶和土壤中的定量限（LOQ）均为0．01mg／kg。采用所建立的方法，测定了山东、湖南2年2地烟叶和土壤中吡唑醚菌酯的残留及消解动态。结果表明：吡唑醚菌酯在山东青岛烟叶和土壤中的半衰期分别为5．9～9．5d和11．1～13．4d；在湖南长沙烟叶和土壤中的半衰期分别为3．1～5．3d和5．4～6．4d。A new method was developed to detect pyraclostrobin residues in tobacco and soil using HPLC with diode-array detector. Tobacco and soil samples were extracted with acetonitrile, cleaned up by Solid Phase Extraction Column （SPE） C18 and PSA columns and detected by High Performance Liquid Chromatography-Diode Array Detector （HPLC-DAD）. Average recoveries of pyraclostrobin fortified at 0.01,0.2 and 2 mg/kg in tobacco leaves ranged from 97.5% to 101.9% and in soil from 93.4% to 101.2% with the relative standard deviations（RSD） of 4.8% to 6.8%, 1.5% to 10.5%,respectively. The limit of quantity （LOQ） was 0. 01 mg/kg in soil and tobacco leaves. Field experiments were performed in Qingdao, Shandong province and Changsha, Hu＇nan province during 2011 to 2012. Using the above method, residue dissipation of pyraclostrobin in tobacco leaves and soil were detected. In Shandong province the results showed that, the half-lives of pyraclostrobin were 5.9 - 9.5 d in green tobacco leaves and 11.1 -13.4 d in soil, respectively, whereas in Hu＇nan province ,the half-lives were 3.1 - 5.3 d in green tobacco leaves and 5.4 - 6.4 d in soil, respectively.

关 键 词：高效液相色谱法 吡唑醚菌酯 烟叶 土壤 残留 消解动态 

分 类 号：O657.72[理学—分析化学]