农药学学报2012，Vol.14Issue(4)：435-439,5.DOI:10.3969/j.issn.1008-7303.2012.04.13
高效液相色谱-串联质谱法测定多杀菌素在甘蓝和土壤中的残留及消解动态
Residue and decline of spinosad in cabbage and soil by high-performance liquid chromatography-tandem mass spectrometry
摘要
Abstract
An efficient, rapid and sensitive analytical method was developed for the determination of spinosad in cabbage and field soil by high-performance liquid chromatography-tandem mass spectrometry ( HPLC-MS/MS). Its decline and residue behavior in cabbage and soil were also'evaluated. Samples were primarily extracted by acetonitrile, cleaned up with PSA dispersive solid phase extraction (DSPE) and finally analyzed by HPLC-MS/MS. The limit of detection and limit of quantification were 6 × 10 -12 g and 0. 005 mg/kg respectively in both cabbage and soil. Average percentage of recovery,RSDs were 87% -95% ,6% - 10% in cabbage and 86% - 100% ,4% -8% in soil respectively. Experiments in Beijing, Anhui and Hunan were conducted in 2011. The results showed decline of spinosad both in cabbage and soil, which were well fitted with the first-order kinetics, and the half-lives were 0. 83 - 1. 16 d and 0. 88 - 1. 17 d, respectively. The final residue experiment were conducted in 2010 and 2011. The results showed that at the recommend dosage and 1. 5 times the dosage [26.25 and 39.38 g(a. i. )/hm2] ,residues in cabbage after 1 day in both treatments were all below MRL value(2.0 mg/kg,by China).关键词
高效液相色谱-串联质谱(HPLC-MS/MS)/多杀菌素/分散固相萃取/甘蓝/残留Key words
high-performance liquid chromatography-tandem mass spectrometry ( HPLC-MS/MS) / spinosad/ dispersive solid-phase extraction (DSPE)/ cabbage/ residue分类
化学化工引用本文复制引用
王凯,李建中,宋祥梅,于丁一,莫汉宏,王会利..高效液相色谱-串联质谱法测定多杀菌素在甘蓝和土壤中的残留及消解动态[J].农药学学报,2012,14(4):435-439,5.基金项目
中国科学院知识创新工程重要方向项目(KZCX2-YW-JS403:KSCX2-EW-G-6). （KZCX2-YW-JS403:KSCX2-EW-G-6）
