烯唑醇免疫亲和色谱柱的制备及其在样品前处理中的应用

摘要

The purified anti-diniconazole antibody was polymerised to hydrolytic tetramethox-ysilane (TMOS) to synthesize the immunosorbent for the immunoaffinity chromatographic (IAC) column specific to diniconazole. The optimized conditions of the IAC were as follows: water as equilibrium and adsorbent medium, 30% and 50% (v/v) methanol aqueous solutions as eluents. The results showed that the dynamic column capacity was up to 125.4 jAg/g of bed volume. The river water and fruit samples spiked with diniconazole were cleaned up and enriched by the IAC, and the diniconazole in eluant was determined by high performance liquid chromatography. The average recoveries (n = 5) of diniconazole in river water sample were 90. 36% - 100. 14% with relative standard deviations (RSDs) of 2. 03% - 6. 08%, and the average recoveries in fruit samples were 85. 55% - 94. 02% with RSDs of 3. 38% - 6. 78%. The IAC cleanup procedure provided an effective pretreatment method for the determination of diniconazole in sample media such as river water and fruits.%将四甲氧基硅烷(TMOS)水解后与烯唑醇抗体聚合,采用溶胶-凝胶法合成了烯唑醇免疫亲和色谱(IAC)柱固定相,并用其制备了对烯唑醇具有特异性亲和力的IAC柱.对IAC柱条件进行了优化,选择超纯水作为吸附与平衡介质,30％～50％(体积分数)甲醇水溶液作为洗脱剂.结果表明:在优化条件下,IAC柱对烯唑醇的动态柱容量达125.4 μ,g/g.在河水样品和水果样品中添加烯唑醇,经IAC柱净化富集,洗脱液采用高效液相色谱检测,河水中烯唑醇的平均回收率为90.369％～100.14％,相对标准偏差(RSD)为2.03％～6.08％；水果中烯唑醇的平均回收率为85.55％ ～ 94.029％,RSD为3.38％～6.78％.本研究为烯唑醇在河水、水果等样品中的残留分析提供了一种新的高效前处理手段.