固相微萃取技术在果蔬农残检测中的应用研究
The Application Research of Solid Phase Microextraction on the Detection of Pesticides Residue in Fruits and Vegetables
邱霞琴 1岳都盛2
作者信息
- 1. 昆山市产品质量监督检验所,江苏昆山215316
- 2. 上海杰星生物科技有限公司,上海201700
- 折叠
摘要
[目的]研究固相微萃取技术在果蔬农残检测中的应用,建立合适的测定果蔬中农药残留的分析方法.[方法]以3-氨丙基三乙氧基硅烷为功能单体,水胺硫磷为模板分子,采用溶胶-凝胶方法制备了分子印迹固相微萃取萃取头,建立分子印迹固相微萃取(MIS-PME)与气相色谱(GC-NPD)联用测定果蔬中5种有机磷的分析方法.[结果]试验得出,制得的分子印迹固相微萃取头对果蔬基质中的目标物具有很高的萃取量.分子印迹固相微萃取-气相色谱法方法的线性范围在μg/kg级别,相关系数大于0.994,检出限在0.01～1.33μg/kg,5次重复加标试验所得RSD在1.77％ ～ 9.28％,在真实样品中的加标回收率为88.5％-107.2％.[结论]分子印迹固相微萃取与气相色谱联用测定果蔬中有机磷的方法简单、快速,无需溶剂,准确度高,具有广阔的应用前景.
Abstract
[Objective] The aim was to study the application of solid phase microextraction in detection of pesticides residue in fruits and vegetables, and establish appropriate analysis method.[Method] With 3-aminopropyltriethoxysilane (APTES) as the functional monomer, isocarbophos as a template, a novel molecularly imprinted solid phase microextraction (MISPME) fiber was prepared by sol-gel technique.The method based on MISPME combined with gas chromatography(GC-NPD) was developed for the determination of organophosphorus (OPPs) in vegetable and fruit samples.[Result] The fiber exhibited high extraction capacity to the target in the real samples.The linear ranges were achieved at the μg/kg levels and the linear correlation coefficients for all analytes were greater than 0.994, detection limits were between 0.01 -1.33 μg/kg, RSD for the 5 repeated standard addition were between 1.77％-9.28％, the recoveries in real samples were 88.5％-107.2％.[Conclusion] The method based on MISPME combined with GC-NPD for the determination of OPPs in vegetables and fruits is simple, rapid, solvent-free and exhibits high accuracy, which has a board application prospect.
关键词
固相微萃取/溶胶-凝胶/气相色谱/有机磷Key words
Solid phase microextraction/Sol-gel technique/Gas chromatography/Organophosphorus引用本文复制引用
出版年
2016
国家科技期刊平台
NSTL
维普
万方数据