混合三模板分子印迹固相萃取柱应用于粮谷中三唑类农药的检测

建立了采用混合三模板分子印迹固相萃取-高效液相色谱法分离检测粮谷样品中3种三唑类杀菌剂残留的方法。以联苯三唑醇、腈菌唑、烯唑醇为混合模板分子,采用本体聚合法合成了具有高选择性的混合三模板分子印迹聚合物,以该聚合物为填料制备混合三模板分子印迹固相萃取柱,并结合高效液相色谱法检测粮谷中联苯三唑醇、腈菌唑、烯唑醇残留。结果表明,以20 mL水为淋洗剂,15 mL甲醇为洗脱剂,并在最佳色谱条件下,联苯三唑醇、腈菌唑、烯唑醇的平均回收率分别为74.0%~82.4%、79.0%~86.2%、77.5%~85.1%,相对标准偏差(RSD)≤4.4%,该混合三模板分子印迹聚合物对3种杀菌剂具有特异性吸附能力,该分析方法可用于样品中三唑类杀菌剂残留的分离检测。

Application of Mixing Three-template Molecularly Imprinted Solid Phase Extraction Column to Determination of Triazole Pesticides in Grains

A mixing three-template molecularly imprinted solid phase extraction column (MISPEC) - high performance liquid chromatography (HPLC) method was developed for simultaneous determination of three triazole fungicide residues in grain samples. The mixing three-template molecularly imprinted polymer (MIP) with high seletivity to bitertanol, myclobutanil and diniconazole was synthesized through bulk polymerization using bitertanol, myclobutanil and diniconazole as mixing three-template molecules. The mixing three-template molecularly imprinted solid phase extraction column was prepared and used coupled with HPLC to detect bitertanol, myclobutanil and diniconazole in grains. The experimental results showed that water of 20 mL as washing agent, methanol of 15 mL as eluent, and under the best chromatographic conditions, the average recoveries of bitertanol, myclobutanil and diniconazole were respectively 74.0%~82.4%, 79.0%~86.2% and 77.5%~85.1% with the relative standard deviations (RSDs, n=5) less than 4.4%. In conclusion, the polymer has a good specificity absorption capacity for the three fungicides, and the analyticalSmethod can be used for the separation and detection of triazole fungicides in samples.