[关键词]
[摘要]
利用虚拟模板分子印迹固相萃取技术对食品中的联苯三唑醇与烯唑醇进行分离富集,并建立高效液相色谱检测方法。以腈菌唑为模板分子,丙烯酰胺(AM)为功能单体,EDMA为交联剂,乙腈为致孔剂,采用本体聚合法制备得到了腈菌唑分子印迹聚合物(MMIP),以此聚合物为固相萃取剂,制备固相萃取柱,对食品中联苯三唑醇和烯唑醇进行分离富集,并采用高效液相色谱法测定其在食品中的残留。采用C18色谱柱分离,以甲醇-水(体积比为90:10)溶液为流动相,紫外检测波长为210 nm,外标法定量。结果表明,联苯三唑醇和烯唑醇的平均回收率分别为89.40~90.88%和81.37~83.26%,RSD分别为1.08~2.04%和1.29~2.52%,检测限均为0.20 μg/g。此聚合物对两种杀菌剂具有良好的吸附能力,拟模板分子印迹固相萃取技术可以用于这两种杀菌剂的分离检测。
[Key word]
[Abstract]
Myclobutanil molecularly imprinted polymer (MMIP) was prepared by bulk polymerization using myclobutanil as template molecule, methacrylate acid (MAA) as functional monomer, ethylene glycol dimethacrylate (EDMA) as crosslinker and acetonitrile as pore-foaming agent. The solid phase extraction (SPE) column was produced with MMIP as SPE agent. Fungicides of Bitertanol and diniconazole in food could be separated and enriched by SPE column, and then residuals were determined by HPLC. The sample was separated by the C18 column with a mobile phase of methanol and water (90:10, V/V) at the rate of 1mL/min and the wavelength was 210 nm. Their contents were quantified by external standard method. The average recoveries of bitertanol and diniconazole were 89.40~90.88% and 81.37~83.26%, respectively. The detection limits were all 0.20 μg/g. RSDs were 1.08~2.04% for bitertanol and 1.29~2.52% for diniconazole. In conclusion, the polymer had a good adsorption capacity for the two fungicides and the virtual template molecularly imprinted solid phase extraction technology could be used for the separation and detection of the two fungicides.
[中图分类号]
[基金项目]
国家科技支撑计划项目(2013BAD10B03),国家自然科学基金项目(31101358),河北省科技支撑计划项目(10276902D)