Urraca Javier L, Marazuela María Dolores, Moreno-Bondi María C
Laboratory of Optical Sensors, Department of Analytical Chemistry, Faculty of Chemistry, Universidad Complutense de Madrid, 28040, Madrid, Spain.
Anal Bioanal Chem. 2006 Aug;385(7):1155-61. doi: 10.1007/s00216-006-0343-3. Epub 2006 Apr 21.
A molecularly imprinted polymer prepared using 1-allylpiperazine (1-ALPP) as the functional monomer, trimethyltrimethacrylate (TRIM) as the crosslinker and the zearalenone (ZON)-mimicking template cyclododecanyl-2,4-dihydroxybenzoate (CDHB) has been applied to the clean-up and preconcentration of this mycotoxin (zearalenone) and a related metabolite, alpha-zearalenol (alpha-ZOL), from cereal and swine feed sample extracts. The extraction of ZON and alpha-ZOL from the food samples was accomplished using pressurized liquid extraction (PLE) with MeOH/ACN (50:50, v/v) as the extraction solvent, at 50 degrees C and 1500 psi. The extracted samples were cleaned up and preconcentrated through the MIP cartridge and analyzed using HPLC with fluorescence detection (lambda (exc)=271/ lambda (em)=452 nm). The stationary phase was a polar endcapped C18 column, and ACN/MeOH/water 10/55/35 (v/v/v, 15 mM ammonium acetate) at a flow rate of 1.0 mL min(-1) was used as the mobile phase. The method was applied to the analysis of ZON and alpha-ZOL in wheat, corn, barley, rye, rice and swine feed samples fortified with 50, 100 and 400 ng g(-1) of both mycotoxins, and it gave recoveries of between 85 and 97% (RSD 2.1-6.7%, n=3) and 87-97% (RSD 2.3-5.6%, n=3) for alpha-ZOL and ZON, respectively. The method was validated using a corn reference material for ZON.
以1-烯丙基哌嗪（1-ALPP）为功能单体、三甲基三甲基丙烯酸酯（TRIM）为交联剂、玉米赤霉烯酮（ZON）模拟模板环十二烷基-2,4-二羟基苯甲酸酯（CDHB）制备的分子印迹聚合物，已应用于从谷物和猪饲料样品提取物中净化和预浓缩这种霉菌毒素（玉米赤霉烯酮）及相关代谢物α-玉米赤霉醇（α-ZOL）。使用甲醇/乙腈（50:50，v/v）作为萃取溶剂，在50℃和1500 psi条件下通过加压液体萃取（PLE）从食品样品中萃取ZON和α-ZOL。萃取后的样品通过分子印迹聚合物柱进行净化和预浓缩，然后使用荧光检测（激发波长λ(exc)=271/发射波长λ(em)=452 nm）的高效液相色谱进行分析。固定相为极性封端的C18柱，以乙腈/甲醇/水10/55/35（v/v/v，含15 mM醋酸铵）为流动相，流速为1.0 mL min⁻¹。该方法应用于分析添加了50、100和400 ng g⁻¹这两种霉菌毒素的小麦、玉米、大麦、黑麦、水稻和猪饲料样品中的ZON和α-ZOL，α-ZOL和ZON的回收率分别为85%至97%（相对标准偏差2.1 - 6.7%，n = 3）和87%至97%（相对标准偏差2.3 - 5.6%，n = 3）。该方法使用ZON玉米标准物质进行了验证。
