硅胶表面修饰添加剂选择性降低卷烟烟气中的苯酚

分别以聚乙烯亚胺（PEI）、十六烷基三甲基溴化铵（CTMAB）对硅胶（SiO2）表面进行修饰,并以苯酚为模板,合成硅胶表面修饰分子印迹聚合物（MIP-SiO2）,制备获得功能添加剂PEI-SiO2、CTMAB-SiO2、MIP-SiO2。按不同剂量分别将功能添加剂加入到卷烟滤嘴中,考察对卷烟主流烟气中苯酚的截留效率。结果表明,各添加剂均可有效降低卷烟烟气中的苯酚释放量。当添加量达到20mg/支时,各功能材料对苯酚的截留效率均超过39%。且添加剂对烟气中苯酚的截留能力大于对烟气中焦油的吸附能力,表明功能添加剂具有选择性降低卷烟烟气中苯酚的作用。     

1-氨基萘印迹聚合物分子识别特性的光谱学研究

采用分子自组装印迹技术合成了一种对1-氨基萘有高度选择性的分子印迹聚合物新材料。应用紫外光谱、红外光谱、X射线光电子能谱和1H核磁共振波谱等研究了印迹聚合物的结合位点和识别机理。结果表明模板分子与功能单体通过氢键作用形成1:1型配合物,配合物的稳定常数K=5.537×104L/mol。1-氨基萘分子氨基上的氮原子是质子接受体,功能单体甲基丙烯酸分子羧基上的氢原子是氢键的质子给予体,是与1-氨基萘形成氢键作用的选择性识别位点。利用平衡吸附试验研究了印迹聚合物的结合特性,表明印迹聚合物对1-氨基萘分子具有特异的识别性能。     

荧光分子印迹膜选择性检测7-氨基-4-甲基香豆素

合成了以7-氨基-4-甲基香豆素为模板分子,聚偏氟乙烯微孔滤膜为支撑介质的分子印迹复合膜.采用荧光光度法,研究了荧光分子印迹膜的吸附动力学、吸附容量和选择性吸附性能.研究表明,该印迹膜对模板分子具有良好的识别功能.     

久效磷分子印迹聚合物分子识别特性的光谱研究

采用分子印迹技术合成了对有机磷农药久效磷有高度选择性的聚合物,通过1H NMR和紫外光谱研究了印迹聚合物的结合机理和识别特性。结果表明,该聚合物通过协同氢键作用形成1∶2型氢键配合物专一地结合久效磷。聚合物红外光谱研究表明,聚合物表面存在可与印迹分子相互作用的官能团。     

甲胺磷分子印迹聚合物的结合机理及其分子识别特性的光谱学研究

采用分子自组装印迹技术合成了一种新的对甲胺磷农药分子有高度选择性的分子印迹聚合物。在预聚合阶段,通过1H NMR,FTIR和UV光谱法研究了分子印迹聚合物的形成机理。结果表明模板分子和功能单体通过协同氢键作用形成1∶2型氢键配合物,配合物稳定常数K＝2.894×106 L2·mol-2,稳定性好。运用红外光谱法研究了印迹聚合物对模板分子的特异性识别作用,进一步表明印迹聚合物通过协同氢键作用特异性地识别模板分子。     

NNAL模拟模板分子印迹聚合物的合成与固相萃取性能

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%．     

氧化石墨烯-分子印迹聚合物在普萘洛尔SERS检测中的应用

分子印迹聚合物(MIPs)是高选择性多孔材料,氧化石墨烯含有较大的的比表面积和丰富的含氧官能团,我们将氧化石墨烯与MIPs复合,结合两者的优势对普萘洛尔进行SERS检测。这种材料实现了对普萘洛尔的特异性吸附,检测极限可低至10-7 mol·L-1。     

磺胺二甲嘧啶分子印迹聚合物制备与光谱特性

本研究以磺胺二甲嘧啶为模板分子,甲基丙烯酸为功能单体,低温紫外引发聚合制备分子印迹聚合物,用紫外光谱法对磺胺二甲嘧啶与甲基丙烯酸的结合作用及磺胺二甲嘧啶印迹聚合物的静态吸附性能和选择性能进行研究,试验结果表明,溶液中的功能单体与印迹分子之间产生了结合作用;与空白印迹聚合物相比,以甲基丙烯酸为功能单体、磺胺二甲嘧啶为模板的分子印迹聚合物展现了较高的结合容量,与其他结构类似的底物磺胺异唑相比,磺胺二甲嘧啶分子印迹聚合物对磺胺二甲嘧啶模板分子显示出明显的选择性和特异性,静态分配系数K_D可达282.3 mg·mL-1,分离因子α可达3.9,并预测磺胺二甲嘧啶分子印迹聚合物结合机理。分析了甲基丙烯酸、二甲基丙烯酸乙二醇酯和磺胺二甲嘧啶分子印迹聚合物的红外谱图,研究结果表明制备的磺胺二甲嘧啶印迹聚合物中CC双键峰很小,并且功能键羧酸键没有明显变化,经交联聚合得到的聚合物确实存在可以同印迹分子相互作用的化学基团。     

光谱法分析晶须表面离子印迹对镉的吸附行为

以Cd(Ⅱ)离子为模板分子,壳聚糖为功能单体,3-缩水甘油醚氧丙基三甲氧基硅烷(KH-560)作为交联剂同时加入一定量的三钛酸钠晶须合成了新型的三钛酸钠晶须表面Cd(Ⅱ) 离子印迹聚合物吸附剂,通过电感耦合等离子体原子发射光谱法(ICP-AES)研究了此离子印迹聚合物对Cd(Ⅱ)的吸附行为; 探讨了酸度、吸附剂用量,静置时间对吸附行为的影响,同时研究了印迹聚合物对Cd(Ⅱ)的吸附动力学和吸附等温线,得出此吸附属Langmuir吸附模型。根据吸附效率系数(K_d)和选择性系数(K)的大小,考察了离子印迹聚合物的吸附选择性。试验结果表明：在最佳优化条件下,离子印迹聚合物对Cd(Ⅱ)的吸附率可达99%以上,最大吸附容量为52.34 mg·g-1,选择性优于空白印迹聚合物,此方法的检出限为0.024 μg·mL-1,相对标准偏差为1.74%(c=1.0 μg·mL-1, n=13)说明此离子印迹聚合物适用于环境中水样的Cd(Ⅱ)的选择性吸附。     

分子印迹流动注射化学发光法测定盐酸强力霉素

研究发现在碱性条件下,盐酸强力霉素对鲁米诺-铁氰化钾体系化学发光反应具有明显的增敏作用,据此建立了分子印迹-流动注射化学发光法定量分析盐酸强力霉素的新方法。以甲基丙烯酸为功能单体、乙二醇二甲基丙烯酸酯为交联剂合成了盐酸强力霉素的分子印迹聚合物。以此分子印迹聚合物为分子识别物质,利用盐酸强力霉素-鲁米诺-铁氰化钾化学发光体系,结合流动注射化学发光分析技术,建立了测定盐酸强力霉素高选择性的分子印迹-流动注射化学发光分析方法。方法的线性范围为9.0×10-7～6.0×10-5 g·mL-1,检出限为3.2×10-7 g·mL-1。对6.0×10-6 g·mL-1的盐酸强力霉素水溶液进行分析,9次平行测定的相对标准偏差为3.5%。利用此方法测定尿样和盐酸强力霉素药片中盐酸强力霉素的含量,结果令人满意。     

水中铜离子的高选择性检测方法

基于铜离子在碱性介质中能极大地增敏鲁米诺-过氧化氢体系的化学发光,结合铜离子印迹固相萃取技术,建立了高选择性地检测铜离子的固相萃取-流动注射化学发光分析法.本实验考察了该铜离子印迹聚合物-聚4-乙烯吡啶的选择性以及稳定性,并将其制备成固相萃取柱,置于流动注射流路中,对样品中的铜离子进行富集分离,用HCl溶液进行在线洗脱,利用化学发光分析法进行铜离子含量的测定.将本法用于合成水样中铜离子的测定,结果比较满意.     

Preparation and Recognition Behavior Characterization of a Moncrotophos Molecularly Imprinted Polymer

In this study, a novel functionalized material was synthesized using moncrotophos as template molecule, methacrylic acid as functional monomer, and ethylene glycol dimethacrylate as cross-linker. The adsorption ability of the imprinted polymer toward moncrotophos was characterized by static adsorption experiments; the results showed that it had higher adsorption capacity than the non-imprinted polymer. Scatchard analysis indicated that the specific binding sites in the prepared material were heterogeneous and could be classified into two distinct groups. For the saturated adsorption capacity, (Q_max1) was 18.76 mg/g due to the high affinity binding sites, and the other saturated adsorption capacity (Q_max2) was 4.66 mg/g due to the low affinity binding sites. The prepared material also offered fast kinetics for adsorption and desorption of moncrotophos. After shaking for 90 min, an adsorption capacity of 4.48 mg/g was obtained. The material exhibited higher selective recognition properties toward moncrotophos than toward structurally related compounds. Thus, it had the potential to be used as a selective sorbent in solid-phase extraction.     

Preparation of an Estriol Surface Imprinted Polymer and its Adsorption Ability Evaluation

A novel molecularly imprinted polymer/magnetic chitosan microsphere (MIP/MCM) was prepared by a surface molecular imprinting technique in combination with a sol–gel process, using estriol as the template, γ-aminopropyltrimethoxysilane as the functional monomer, tetraethoxysilicane as the cross-linker, and magnetic chitosan as the support material. The adsorption ability and selectivity of the polymeric material toward estriol were evaluated. The results indicated that the prepared material had higher adsorption capacity and selectivity toward estriol than the non-imprinted polymer/MCM. The theoretical maximum adsorption capacity (Q _max) was 8.13 mg g^?1, and the equilibrium dissociation constant (K _d) was 625.0 mg mL^?1. The functionalized material had fast uptake kinetics, 83.64% of the saturated adsorption capacity was obtained within a period of 60 min, and the adsorption almost reached equilibrium within 90 min. This prepared material has potential to be used as a sorbent in solid-phase extraction (SPE) to enrich trace estriol in samples.     

SPME/GC-MS分析冷水花的挥发性成分

利用固相微萃取/气相色谱-质谱（SPME/GC-MS）联用技术分析冷水花挥发性化学成分。共鉴定出61个化学成分,占总挥发性成分的98.42%。冷水花挥发性化学成分主要是1-甲基-5-甲烯基-8-（1-异丙基）-[s-（E,E）]-1,6-环癸二烯（20.03%）,石竹烯（13.38%）,1-萘胺（5.27%）,愈创兰油烃（5.20%）,N-（4-羟苯基）-丁酰胺（5.12%）,α-法呢烯（4.73%）,1-甲基-1-乙烯基-2,4-二丙烯基-环己烷（4.59%）等。     

A facile method for grafting of bisphenol A imprinted polymer shells onto poly(divinylbenzene) microspheres through precipitation polymerization

Core-shell structured polymers are usually prepared by “grafting to” or “grafting from” techniques, wherein polymer supports were first modified by vinyl bonds or initiators. Success can be immediate, but more often a learning curve needs to be traversed. In this paper, direct grafting bisphenol A imprinted polymer onto poly(divinylbenzene) microspheres through precipitation polymerization is introduced. The obtained microspheres were characterized by SEM, TEM, FTIR and BET. Firstly, mono-disperse poly(divinylbenzene) microspheres of 3 μm in size were prepared by precipitation polymerization. The solvent for grafting was then optimized and it was found that the mixtures of toluene and acetonitrile (30/70, v/v) were ideal choice from the image and structure analysis of the shells. Shells of different thickness (270-840 nm), depending on the concentrations of monomers in the precursor, were then directly grafted to the microspheres by a reactive, entropic capture mechanism. The recognition ability of the microspheres was evaluated by solid-phase extraction and clear selectivity showed toward bisphenol A. The leak of bisphenol A was not found after extraction and thus these core-shell structured imprinted polymers are believed to have potential applications in trace analysis area.     

Synthesis, characterization and evaluation of uniformly sized core–shell imprinted microspheres for the separation trans-resveratrol from giant knotweed

A novel core–shell molecularly imprinting microspheres (MIMs) with trans-resveratrol as the template molecule; acrylamide (AA) as functional monomer and ethylene glycol dimethacrylate (EGDMA) as cross-linker, was prepared based on SiO₂ microspheres with surface imprinting technique. These core–shell trans-resveratrol imprinted microspheres were characterized by infrared spectra (IR), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), and high performance liquid chromatography (HPLC). The results showed that these core–shell imprinted microspheres, which take on perfect spherical shape with average shell thickness of 150 nm, exhibit especially selective recognition for trans-resveratrol. These imprinted microspheres were applied as solid-phase extraction materials for selective extraction of trans-resveratrol from giant knotweed extracting solution successfully.     

Determination of arsenic species in mainstream cigarette smoke based on inductively coupled plasma mass spectrometry

In this work, arsenic species in mainstream cigarette smoke condensates was systemically studied with inductively coupled plasma mass spectrometry. A single particle inductively coupled plasma mass spectrometry was utilized for analysis of the physical forms of arsenic, and no particle arsenic was observed in mainstream cigarette smoke condensates. The solvent extraction experiments proved that the water-soluble arsenic was the main species in mainstream cigarette smoke condensates, which was consistent with the result of single particle inductively coupled plasma mass spectrometry. Furthermore, speciation of arsenite, arsenate, monomethylarsonic acid, and dimethylarsinic acid was investigated using high performance weak anion exchange chromatography coupled with inductively coupled plasma mass spectrometry detection. The developed high performance liquid chromatography coupled inductively coupled plasma mass spectrometry method was successfully applied to the determination of arsenic species in mainstream cigarette smoke condensates with satisfactory recoveries. Four arsenic species were detected in the mainstream cigarette smoke condensates from four brands of commercial available cigarettes, and there was a great difference between the arsenic content and composition among the different brands of cigarettes. It is found that arsenate was the main species in all tested cigarette samples.