摘要
以三唑酮为模板分子,三氟甲基丙烯酸为功能单体,乙二醇二甲基丙烯酸酯为交联剂,合成了对三唑类农药具有高选择性的分子印迹聚合物。将印迹聚合物作为固相萃取填料,优化分离、富集三唑类农药的最优上样、淋洗和洗脱条件。结合液相色谱串联质谱法,实现了果蔬样品中20种三唑类杀菌剂的高通量特异性检测。对样品前处理过程中的加标回收率进行了考察,并对比了分子印迹固相萃取和ENVI-Carb/SPE小柱的基质效应。结果表明:在1.0,2.0和10.0μg/kg加标水平下,三唑类农药的回收率在81.0%~109.7%之间,相对标准偏差小于12.6%,基质效应在91.1%~121.8%之间。方法灵敏、准确度高,与ENVI-Carb/SPE小柱相比,能更有效减弱基体效应。
Molecularly imprinted polymers (MIPs) with high selectivity using triadimefon as template, trifluoromethyl acrylic acid (TFMAA) as to triazoles functional residues were prepared monomer and ethylene glycol dimethacrylate (EGDMA) as cross-linker. The MIPs were applied as solid phase extraction materials. The optimum loading, washing and eluting conditions for molecularly imprinted solid phase extraction (MISPE) were established to obtain high selectivity and sensitivity. Coupled with LC-MS/MS, a high throughput and selective method was developed for simultaneous determination of 20 triazole pesticides in vegetables and fruits. The spiked recovery was investigated and the matrix effects were compared between MISPE and ENVI-Carb/PSA SPE columns. The results showed that the pesticide recoveries were in the range of 81.0% -109.7% with RSD lower than 13% at 1.0, 2.0 and 10.0μg/kg spiked levels, and the matrix effect was in the range of 91.1% -121.8%. Compared with ENVI-Carb/PSA SPE columns, MISPE exhibited selective binding properties for triazoles and the matrix effect was significantly decreased.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2014年第2期227-232,共6页
Chinese Journal of Analytical Chemistry
基金
国家质检总局科研项目(No.2009IK166)
安徽省科技攻关项目(No.12010402c205)资助
关键词
分子印迹聚合物
固相萃取
三唑类农药
Molecularly-imprinted polymers
Solid phase extraction
Triazoles pesticides
Carrot
Pear