摘要
建立了分散固相萃取-分散液液微萃取与气相色谱/质谱联用测定玉米和大米中痕量氟虫腈及其代谢物残留的分析方法。使用乙腈和水混合溶液作为萃取溶剂,盐析后,提取液经N-丙基-乙二胺硅烷固相萃取材料（PSA）作为吸附剂后,采用分散液液微萃取步骤将目标物从到微量四氯乙烯中。对影响分散液液微萃取效率的因素,包括萃取溶剂种类及体积、盐等条件进行了优化。在0.02~1μg/m L浓度范围内,线性关系良好（r≥0.9987）。在玉米和大米样品中氟虫腈添加浓度为1.0~25.0μg/g时,平均回收率在70.4%~95.1%之间,相对标准偏差（n=5）在2.6%~12%之间,以最低添加浓度1μg/kg作为定量限。
A gas chromatograph-mass spectrometer（ GC-MS） method for the determination of fipronil and metabolite pesticide residues in corn and rice samples was established using dispersive solid-phase extraction and dispersive liquid-liquid microextraction（ DLLME） as sample preparation methods. The samples were extracted with acetonitrile and water solution,after the salting out procedure,the extract was purified with primary secondary amine（ PSA） sorbent. Factors affecting the extraction efficiency of DLLME such as type and volume of extraction solvent,and salting effect were investigated. The calibration curves were linear in the range of 0. 02~ 1 μg / m L（ r ≥0. 9987）. The recoveries ranged from 70. 4% to 95. 1% at fortified levels of 1. 0 ~ 25. 0μg / kg with RSD varied from 2. 6 to 11. 1%. The limits of quantification based on the lowest fortification level were 1 μg / kg. The proposed method has the advantage of simple operation,quickness and high sensitivity. The proposed method is applicable for the analysis of fipronil and its metabolite residues in corn and rice samples.
出处
《分析试验室》
CAS
CSCD
北大核心
2016年第4期386-389,共4页
Chinese Journal of Analysis Laboratory
基金
国家自然科学基金项目(31301694)
北京市农林科学院青年基金项目(QNJJ201310)资助
关键词
分散固相萃取
分散液液微萃取
气相色谱-质谱
氟虫腈
玉米
大米
Dispersive liquid-liquid microextraction
Dispersive solid-phase extraction
Gas chromatography-mass spectrometer
Fipronil
Corn
Rice
