高效液相色谱法检测烟草中噻虫嗪残留及消解动态  

Residue and dissipation of thiamethoxam in tobacco by high performance liquid chromatography

作　　者：宋超[1] 李海萍 刘万峰 陆伟 徐光军[1] 徐金丽[1] 郑晓[1] 李义强[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]青岛市农业环保能源工作站,山东青岛266000 [3]湖南中烟工业有限责任公司,长沙471000 [4]山东省烟草专卖局,济南250100

出　　处：《农药学学报》2014年第4期477-482,共6页Chinese Journal of Pesticide Science

基　　金：国家烟草专卖局项目(TS-06-20110039);农业行业财政专项(201203091)

摘　　要：建立了高效液相色谱法检测鲜烟叶和干烟叶中噻虫嗪残留量的方法。样品经乙腈提取，Cleanert NH2-SPE固相萃取柱净化，高效液相色谱．紫外检测器（HPLC—UV）检测，外标法定量。结果表明：在0．01～5mg／kg添加水平下，鲜烟叶中噻虫嗪的平均回收率为92％～95％，相对标准偏差（RSD）为4．5％-9．2％，定量限（LOQ）为0．01mg!kg；在0．05～5mg／kg添加水平下，干烟叶中噻虫嗪的平均回收率为91％～94％，RSD为5．9％-6．8％，LOQ为0．05mg／kg。采用所建立的方法，测定了山东、湖南2年2地烟叶样品中噻虫嗪的消解动态及最终残留量。结果表明：噻虫嗪在烟叶中的半衰期为1．3～8．1d；按照噻虫嗪有效成分用量18．9和28．4g／hm2，于烟草现蕾初期．成熟期对水喷雾施药2—3次，距末次施药7d后，山东、湖南2年2地烟叶样品中噻虫嗪残留量为0．05～0．80mg／kg，均低于国际烟草合作研究中心（CORESTA）指导性残留限量标准规定的MRL值（5．0mg／kg）。A new method using high performance liquid chromatography-ultraviolet detector （HPLC- UV） was developed to analyze thiamethoxam residue in fresh tobacco leaves and cured tobacco leaves.Samples were extracted with acetonitrile, cleaned up by solid phase extraction column （SPE）, and detected by HPLC-UV with quantification by external standard method. The result shows that when thiamethoxam was spiked at 0. 01 - 5.0 mg/kg levels in fresh tobacco leaves and 0. 05 - 5.0 mg/kg levels in cured tobacco leaves, the average recoveries of thiamethoxam were 92% -95% and 91% - 94%, with relative standard deviations （RSDs） of 4.5% - 9.2% and 5.9% - 6.8%. The limit of quantification （LOQ） of this method was 0. 01 mg/kg in fresh tobacco leaves and 0. 05 mg/kg in cured tobacco leaves. Field experiments were performed in Qingdao, Shandong Province and Changsha, Hu＇nan Province. Dynamic resuks showed the half-live of thiamethoxam in green tobacco leaves was 1.3 - 8.1 d. When sprayed with 2 and 3 times dosages of 18.9 and 28.4 g a. i./hm2 at the bud stage to maturity stage of tobacco, residues in cured tobacco leaves after 7 days in all treatment ranged from 0.05 to 0.80 mg/kg, which were all below MRL value set by CORESTA （5.0 mg/kg）.

关 键 词：高效液相色谱 烟叶 噻虫嗪 残留 消解动态 

分 类 号：TQ450.2[化学工程—农药化工]