固相萃取柱净化-经济学家.pdf

222 2015, Vol.36, No.20 食品科学 ※安全检测 固相萃取柱净化-高效液相色谱法测定小麦中 脱氧雪腐镰刀菌烯醇 罗颖鹏，陈正行，王 韧，罗小虎，李永富，李亚男，邵慧丽，王 莉* （江南大学食品学院，粮食发酵工艺与技术国家工程实验室，食品科学与技术国家重点实验室，江苏无锡 214122 ） 摘  要：建立固相萃取-高效液相色谱对小麦中脱氧雪腐镰刀菌烯醇（deoxynivalenol ，DON ）进行测定的方法。从 提取溶剂、净化方式、流动相组成以及流动相流速等条件优化DON检测方法。结果表明，当样品提取溶剂为乙腈- V V V V 水（84 ∶16， / ），Bond Elut Mycotoxin 固相萃取柱净化，流动相组成为乙腈-水（6 ∶94， / ），流速为0.9 mL/min 时，DON检测结果最好，该检测方法的DON 回收率达到90.12%～106.25%，日内和日间相对标准偏差分别为4.51% 和6.12%。该方法快速、准确，重复性好，稳定性高，适合DON污染小麦样品的大批量检测。 关键词：脱氧雪腐镰刀菌烯醇；小麦；高效液相色谱；固相萃取；检测 Determination of Deoxynivalenol in Wheat Grains by HPLC Using Solid-Phase Extraction Cleanup Column * LUO Yingpeng, CHEN Zhengxing, WANG Ren, LUO Xiaohu, LI Yongfu, LI Yanan, SHAO Huili, WANG Li (National Engineering Laboratory for Cereal Fermentation Technology, State Key Laboratory of Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi 214122, China) Abstract: Deoxynivalenol (DON) is a ubiquitous mycotoxin present in cereal grains such as wheat and corn. This mycotoxin causes huge damage to human and animal health. This study optimized the experimental conditions including extraction solvent, cleanup column, composition and flow rate of mobile phase for DON detection by high-performance liquid chromatography (HPLC) after solid-phase extraction (SPE) cleanup. The optimized HPLC method was established when the V V extraction was performed using a mixture of acetonitrile (ACN) and water (84:16, / ) followed by SPE cleanup on a Bond