分子印迹固相萃取-液相色谱-质谱法测定果蔬中20种三唑类农药残留  

Selective Detection of 20 Triazoles Residues in Food Uusing Molecularly Imprinted Solid Phase Extraction coupled with Liquid Chromatography Tandem Mass Spectrometry

作　　者：胡艳云[1,2] 徐慧群[1] 姚剑[1] 吕亚宁[1,2] 宋伟[1,2] 李文静[3] 韩芳[1,2] 郑平[1,2] 

机构地区：[1]安徽出入境检验检疫局,合肥230022 [2]食品安全分析与检测安徽省重点实验室,合肥230022 [3]安徽大学化学化工学院,合肥230039

出　　处：《分析化学》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

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.

关 键 词：分子印迹聚合物 固相萃取 三唑类农药 

分 类 号：TS255.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]