本文建立了同时分离检测粮谷样品中4种三唑类杀菌剂的分子印迹固相萃取膜-高效液相色谱法。采用自制的联苯三唑醇分子印迹固相萃取膜对粮谷中的联苯三唑醇、三唑酮、烯唑醇和戊唑醇残留进行分离富集，并采用高效液相色谱法测定其在粮谷样品中的残留。试验对淋洗剂、洗脱剂的种类和用量以及检测条件进行了优化。以5 mL水为淋洗剂，3 mL甲醇为洗脱剂，使用C18色谱柱，以甲醇-水（体积比为82:18）溶液为流动相，紫外检测波长为210 nm，外标法定量。结果表明，4种杀菌剂平均回收率在84.2%~98.1%之间，相对标准偏差（RSDs）在1.2%~2.7%之间（n=5）。该分子印迹固相萃取膜不仅对样品净化效果好，而且对4种杀菌剂特异吸附能力强。该方法能高效、快速、灵敏检测粮谷样品中三唑类杀菌剂。

A molecularly imprinted solid-phase extraction membrane (MISPEM) coupled with high-performance liquid chromatography (HPLC) method for the simultaneous determination of four triazole fungicides in grain samples was developed. Residues of bitertanol, triadimefon, diniconazole, and tebuconazole in grains were separated and enriched using the self-prepared MISPEM. These enriched residues were subsequently analyzed by HPLC. Process characteristics such as washing agents, the type and amount of eluents, and the detecting conditions were optimized. For this process, using 5 mL water and 3 mL methanol as the washing agent and eluent, respectively; the samples were separated with a C18 column, using a mobile phase of methanol and water (82:18, V/V). The separation was quantified using an external standard method, by detection at a wavelength of 210 nm. The average recovery rates of the four fungicides were discovered to be between 84.2% and 98.1%; the relative standard deviations (RSDs) ranged from 1.2% to 2.7% (n = 5). The MISPEM showed a good cleansing effect on the samples, as well as strong adsorption capacities for the four fungicides. These results suggest that this method can be used in the efficient, sensitive, and rapid determination of triazole fungicides in grain samples.

河北省科技支撑计划项目（14227504D，14236602D-13）