【作者】 李魏嶙；

【导师】 李莉；

【作者基本信息】 新疆医科大学 ， 药学， 2008， 硕士

【摘要】 目的:制备异丙酚分子印迹固相萃取柱和适合前处理异丙酚血样的膜分离装置,建立快速、连续、实用的异丙酚血样前处理方法,并把膜分离装置和异丙酚分子印迹固相萃取柱结合起来,对之前课题组研制的异丙酚光纤荧光检测系统系统进行改进。方法:分别用热聚合法和紫外光照射法合成异丙酚分子印迹聚合物,用相转化法和紫外光引发原位聚合法制备异丙酚分子印迹膜,考察聚合物的性能、膜的形态、聚合反应机理及印迹聚合物对血浆中异丙酚的吸附;用所得聚合物制备分子印迹固相萃取柱,优化萃取柱的活化、淋洗和洗脱条件,比较了C18柱和分子印迹柱对异丙酚血浆样品的前处理效果;利用膜分离的方法来分离全血中的异丙酚,筛选出合适的膜、萃取液和泵速;把膜分离、分子印迹固相萃取和课题组之前研究的异丙酚光纤荧光检测系统结合起来,分析异丙酚的血药浓度。结果:(1)印迹聚合物选择性的结合异丙酚;紫外光照射法制得的印迹聚合物对异丙酚的结合量高于热聚合法制得的印迹聚合物;聚合温度越高,聚合反应进行的越完全,相应的聚合物的溶胀越差,表现为识别能力的降低;异丙酚和功能单体甲基丙烯酸以1:1的比例、氢键的方式缔合;当紫外灯离印迹膜5cm时,预聚溶液快速、完整的成膜;印迹聚合物从血浆中吸附出了的部分异丙酚。(2)以正己烷为活化剂,正己烷:甲苯(9:1)为淋洗剂,甲醇为洗脱剂后,分子印迹柱处理异丙酚样品的累计回收率高达99.94%;相比于C18固相萃取柱来说,MIP作为SPE的萃取材料前处理系列浓度的异丙酚血样,其线性和准确性都较好。(3)利用膜分离的方法来萃取全血中异丙酚的过程中,异丙酚血样浓度在1～20μg.ml-1范围内,选用聚醚砜超滤膜,血浆为透析液,5rpm的泵速和2min的透析时间,透析的平均回收率为25.50%,SD为0.54%。(4)选择100mg的聚合物量和5bar的进样压力在改进的异丙酚光纤荧光检测系统上分析全血中异丙酚的浓度,每分析一份样品仅需4.8分钟。结论:膜分离装置结合分子印迹固相萃取柱可以在线、快速的前处理异丙酚的全血样品,对血液无“损伤”,这对异丙酚光纤荧光检测系统来说是一个巨大的改进。更多还原

【Abstract】 Objective: To prepare propofol molecular imprinting solid phase extraction columns and membrane separation device for pre-treatment propofol samples, establish a rapid, continuous and practical approach for pre-treating propofol blood samples,improve the fiber-optical fluorescence detection system developed by item team for propofol with membrane separation device integrated with molecularly imprinted solid phase extraction columns. Method: Synthesis of molecularly imprinted polymers with propofol as template by thermal and UV polymerization,preparation of propofol molecularly imprinted membrane with phase inversion and UV-triggered in-situ polymerization, study of the performance of polymers, the morphology of membrane, the reaction mechanism of polymerization and the adsorption of propofol in plasma adsorbed by Imprinted Polymers ;preparation of molecularly imprinted solid phase extraction columns with polymers, and optimization of activation, washing and elution conditions of extraction columns,compareation of the effects of propofol plasma samples pretreated by C18 columns and molecularly imprinted columns; separation of propofol in the whole blood with membrane separation approach, and selection of suitable membrane, extraction agent and pump speed;membrane separation and molecularly imprinted solid phase extraction integrated with fiber-optical fluorescence detection system developed by item team for propofol was used to analyze the concentration of propofol in blood. Results: (1) Imprinted polymers binded to propofol selectively; binding capacity of imprinted Polymers prepared by UV polymerization was higher than that prepared by thermal polymerization;the higher polymerization temperature, the more completive polymerization reaction, the corresponding poorer swell of the polymers, and the ability of identification decreased; propofol binded to functional monomer methyl acrylate with hydrogen bond and 1:1 ratio,when the distanse between UV lamps and imprinted membrane was 5 cm , prepolymer solution formated membrane quickly and completely; imprinted Polymer adsorbed part of propofol in plasma. (2) When n-hexane as activation, hexane: toluene (9:1) as eluent, methanol as eluting agent,the cumulative recovery of propofol samples treated by molecularly imprinted columns was 99.94%, the linear and accuracy of pre-treatment of series concentrations of propofol in blood with MISPE were better than that of C18 columns. (3)In the process of extracting propofol in whole blood with membrane separation approach, when the concentration of propofol in blood was 1 to 20μg.ml-1, the selection of polyethersulfone membrane for mesomerism and plasma for dialysis fluid, 5 rpm for the pump speed and 2 min for dialysis time, the average recovery rate of dialysis was 25.50%, SD was 0.54%. (4) 100 mg of polymer and 5 bar pressure of injection were choosen to analyze the concentration of propofol in whole blood with improved fiber-optical fluorescence detection system for propofol, only 4.8 minutes for analysis of every sample. Conclusion: Membrane separation device integrated with molecularly imprinted solid phase extraction columns can treat propofol samples in the whole blood online and rapidly, no blood "injury" ,this was a great improvement of fiber-optical fluorescence detection system for propofol.更多还原