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Synthesis and Solid Phase Extraction Performance Study of NNAL-specific Molecularly Imprinted Polymers Using Dummy Templates
Zhi-dan Zhang,Sai-jing Zheng,Jun Yang*,Wei-miao Wang,Bai-zhai Liu,Xiao-lan Zhu
Author NameAffiliationE-mail
Zhi-dan Zhang Department of Chemistry, University of Science and Technology of China, Hefei 230026, China  
Sai-jing Zheng Key Laboratory of Cigarette Smoke Research of China National Tobacco Corporation, Shanghai 200082, China  
Jun Yang* Department of Chemistry, University of Science and Technology of China, Hefei 230026, China yjun8202@ustc.edu.cn 
Wei-miao Wang Key Laboratory of Cigarette Smoke Research of China National Tobacco Corporation, Shanghai 200082, China  
Bai-zhai Liu Key Laboratory of Cigarette Smoke Research of China National Tobacco Corporation, Shanghai 200082, China  
Xiao-lan Zhu Department of Chemistry, University of Science and Technology of China, Hefei 230026, China  
Abstract:
Dummy molecularly imprinted polymers (DMIPs) for 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol (NNAL) were produced using three structural analogues as dummy template molecules. The chosen analogues were 4-(acetymethylamino)-1-(3-pyridyl)-butanol, 4- (methylamino)-1-(3-pyridyl)-1-butanol, and 1-(3-pyridyl)-1,4,-butanediol. The molecular recognition characteristics of the produced polymers were evaluated by X-ray photoelec-tron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FT-IR). Interactions between NNAL and methacrylic acid should be cooperative hydrogen bonds while the ni-trogen atom of the pyridine ring and the oxygen atom of the nitroso group in NNAL are two of the hydrogen-bond acceptors. It was further demonstrated that DMIP synthesized by 4-(acetymethylamino)-1-(3-pyridyl)-butanol had the best binding performance by XPS and FT-IR. Then dummy molecularly imprinted solid phase extraction (DMISPE) was developed for the determination of the analyte using the hit polymer as the sorbing material. Under optimal conditions, the recovery of NNAL dissolved in standard solution reached 93%. And the investigated polymer exhibited much higher binding of NNAL when nicotine was acted as the competitive molecule. Also the proposed method was applied to the measurement of NNAL spiked in blank urine samples with recoveries ranging from 87.2% to 101.2%.
Key words:  Molecularly imprinted polymer, Dummy template, 4-(Methylnitrosamino)-1-(3-pyridyl)-1-butanol, Solid phase extraction
FundProject:
NNAL模拟模板分子印迹聚合物的合成与固相萃取性能
张志丹,郑赛晶,杨俊*,王维妙,刘百战,朱晓兰
摘要:
以三种4-甲基亚硝胺-1-(3-吡啶基)-1-丁醇(NNAL)的结构类似物即4-(N-甲基-N-乙酰基)-1-(3-吡啶基)-1-丁醇、4-(N-甲基)-1-(3-吡啶基)-1-丁醇、1-(3-吡啶基)-1,4-丁二醇为模拟模板分子,甲基丙烯酸(MAA)为功能单体,通过自组装技术制备了对NNAL具有良好识别能力的印迹聚合物.通过X射线光电子能谱和红外光谱研究了NNAL和MAA之间的相互作用,结果表明NNAL和MAA可以通过氢键协同作用形成1:2型配合物.吡啶上的N和亚硝基中的O是形成氢键作用的两个选择性识别位点.XPS和IR进一步揭示出由4-(N-甲基-N-乙酰基)-1-(3-吡啶基)-1-丁醇制备得到的印迹聚合物对NNAL有最佳的识别性能.此外,实验研究了该聚合物作为固相萃取填料分离、净化NNAL的最佳条件.当采用水溶液上样,分别以0.5 mL水、1 mL甲苯、1 mL甲苯/二氯甲烷(9:1)、1 mL甲苯/二氯甲烷(4:1)淋洗,3£1 mL甲醇洗脱时,NNAL在分子印迹固相萃取柱上的回收率达到93%.以尼古丁为竞争分子的选择性实验进一步证明该材料有很好的特异性识别能力.同时在不同加标水平尿液(500 pg/mL,1000 pg/mL,2000 pg/mL)的回收实验中,NNAL的回收率范围为87.2%~101.2%,精密度值均低于7.1%.
关键词:  分子印迹聚合物,模拟模板,4-甲基亚硝胺-1-(3-吡啶基)-1-丁醇,固相萃取
DOI:10.1063/1674-0068/26/03/361-368
分类号: