藉分子印迹固相萃取联用技术对痕量物质的识别

【作者】 黄招发；

【导师】 汤又文；

【作者基本信息】 华南师范大学 ， 物理化学， 2005， 硕士

【摘要】 在临床上,很多药物使用不当会导致副作用,甚至中毒致死。对病人用药的临床监测相当重要,体液中痕量药物的测定由于基体干扰因素使分离富集必不可少。固相萃取作为一种新型的分离富集方法,因其简单、便宜、有机溶剂用量少、易实现自动化等优点,正日益取代传统的液液萃取。但由于普通的固相萃取是用烷基硅、共聚物、石墨化炭等作吸附材料,它们的选择性不够高,使固相萃取的广泛应用受到很大限制。分子印迹技术由于其构效预定性、特异识别性和广泛实用性日益受到人们的重视。分子印迹技术和固相萃取联用是分子印迹技术最有可能实现商业化的应用。 本文实验了头孢硫脒分子印迹聚合物制备的各种条件,发现对酸性的模板分子头孢硫脒,用碱性的功能单体4-乙烯基吡啶比酸性的功能单体甲基丙烯酸具有更高的特异性吸附;模板分子和功能单体比例为1:6制备的分子印迹聚合物吸附效果比1:4和1:8要好;用甲苯作致孔剂比用乙腈作致孔剂制备的聚合物有更大的网状结构,能更快的吸附底物。 并将分子印迹技术和固相萃取联用,实验了头孢硫脒分子印迹聚合物作为固相萃取材料对模板分子的萃取条件。并将其应用于实际样品,分离富集人血液中的头孢硫脒,得到满意的结果。 同时,通过紫外可见光谱实验和结合量实验推断了头孢硫脒同功能单体4-乙烯基吡啶之间的作用力;动力学实验、Scatchard方程分析初步探讨了模板分子和功能单体的作用机理;通过固相萃取装载液、洗脱液等条件的变化进一步论证了分子印迹的原理。 本文还用悬浮聚合法合成了艾司唑仑分子印迹聚合物,并用作固相萃取填充料,通过装载液、淋洗液、洗脱液的优化,建立了一种分离富集艾司唑仑及其类似物的方法,探讨了艾司唑仑分子印迹聚合物对底物的吸附机理。更多还原

【Abstract】 The side-effect or toxicosis caused by improper use of medicine makes it important to screen the drug clinically. Solid-phase extraction (SPE) is gradually substituting for the traditional liquid-liquid extraction (LLE) for its simplicity, low-in-price, less organic solvent, easily automation, etc. The ordinary SPE sorbents such as alkyl-silica, copolymers, graphitized carbon are not highly selective which hinders its development. The molecular imprinted technique is taken more and more care for its predetermination, selective recognition, widely use. Molecularly imprinted solid phase extraction is the most possibly commercialized technology at present application of molecular imprinted technique.We found that the cefathiamidine (CTM) imprinted polymer shows higher selectivity which use the basic 4- vinylpyridine (4-VP) as monomer comparing to the methacrylic acid (MAA), stronger affinity when the ratio between the template and the monomer is 1:6 rather than 1:4 or 1:8, faster rebinding which use toluene as porgen in place of acetonitrile.The molecularly imprinted polymer was used as adsorbents of solid phase extraction. The best conditions were found and the sample in human blood spiked with analyte is practiced. The result was rather good.Moreover, we have discussed the binding and rebinding mechanism by UV-vis spectrum, binding experiment, kinetic experiment, Scatchard formula, SPE procedure, etc.In this article, a separation method of Estazolam from the analogs via molecularly imprinted solid phase extraction was established. The polymer was synthesized by suspension polymerization, and the conditions of solid phase extraction such as loading solvent, washing and eluent were optimized. The binding and rebinding mechanism of Estazolam imprintedpolymer was discussed too.The results illustrated that the molecularly imprinted solid phase extraction is a good manner for the sample cleaning before detected by HPLC, and is expected to apply in clinic detecting diagnosis and treatment.更多还原