以赛庚啶为模板分子,甲基丙烯酸为功能单体,乙二醇二甲基丙烯酸酯为交联剂,通过优化致孔剂、单体及模板与单体摩尔比等因素,合成了对赛庚啶具有高选择性的分子印迹聚合物,其表面积达24.9 m^2/g。制备的印迹聚合物固相萃取小柱(MISPE)依次以甲醇和水活化小柱,水溶液上样,水和甲醇依次洗涤,氨化甲醇(5∶95,V/V)洗脱,赛庚啶在制备MISPE小柱上的回收率为94.0%,而非分子印迹小柱(NISPE)的回收率仅为38.9%;MISPE结合赛庚啶的容量达8.8 mg/g,印迹因子约为2.32。在优化的固相萃取条件下,10 mg/L赛庚啶、阿米替林、磺胺嘧啶和甲氧苄啶混合标准溶液上样,进行选择性实验。以0.05%戊烷磺酸钠溶液和乙腈为流动相,梯度洗脱,在MISPE小柱上,与CYP化学结构差异较大的磺胺嘧啶和甲氧苄啶回收率均小于10%,结构相似的阿米替林回收率达70%,赛庚啶回收率大于90%;4种分析物在NISPE小柱上的回收率均小于30%。制备的MISPE小柱应用于畜禽饮用水样中赛庚啶的分离富集和分析测定,方法回收率为80.5%-97.7%,检出限达0.01 mg/L。
Using cyproheptadine( CYP) as template molecule,methacrylic acid( MAA) as monomer, ethylene glycol dimethacrylate( EGDMA) as cross-linker,molecularly imprinted polymers( MIP) with high selectivity to cyproheptadine( CYP) were prepared by the optimization of porogen,monomer,and the mole ratio of monomer to template. The specific surface area of the prepared polymers was 24. 9 m^2/ g. The recovery of CYP was above 94. 0% when the following procedure was applied to the cartridge of MIP as adsorptive material: conditioning with methanol and water,loading with water,washing with water and methanol,and eluting with methanol-ammonia(95∶ 5,V / V). As a control,the recovery of CYP on non-imprinted polymers cartridge( NISPE) was only 38. 9%. The binding capacity of the molecularly imprinted solid phase extraction(MISPE) towards CYP found to be about 8. 8 mg of CYP/g polymers and the imprinting factor(IF) was about 2. 32. Under optimal conditions, a mixed standard solution of CYP, amitriptyline, sulfadiazine and trimethoprim( 10 mg / L each) was uploaded on the MISPE and NISPE for selectivity experiment. The gradient elution was used by using 0. 05% sodium pentanesulfonate solution( A)-acetintrile( B) as a mobile phase. The recoveries on the MISPE for sulfadiazine and trimethoprim( different structure with CYP) were less than 10%,however,the recovery for the similar structural amitriptyline was more than 70%,and the recovery more than 90% for CYP. All the recoveries on the NISPE for four analytes were less than 30%. This new MISPE cartridge was applied to extract and enrich CYP in livestock drinking water sample,and the recoveries of CYP ranged from 80. 5%- 97. 7%,and the limit of detection( LOD) was 0. 01 mg / L.