双模板分子印迹聚合物在奶粉检验中的应用研究

采用本体聚合法制备三聚氰胺(MEL)与双氰胺(DCD)双模板分子印迹聚合物(MEL/DCD-MIPs),将其作为固相萃取介质,实现了奶粉中MEL与DCD富集与纯化,建立了奶粉中两种物质同时检测的方法。通过热力学、选择性和动态结合试验表明,与单模板分子印迹聚合物相比,双模板分子印迹聚合物由于双模板-功能单体分子间的多位点协同作用而有更好的印迹效应,对MEL和DCD结合能力高于结构类似物三聚氰酸(CYA)。固相萃取试验显示,MEL/DCD-MIPs可以从市售奶粉中选择性地分离、富集MEL与DCD,对MEL与DCD的加样回收率分别为93.1%~100.1%和75.7%~82.5%,RSD均小于5.2%。所制得的MEL/DCD-MIPs可应用于奶粉等食品中氰胺类物质的检测。     

小分子甲苯印迹聚合物的制备及其吸附性能研究

利用甲苯的致孔效应,以甲苯作为模板分子,以甲基丙烯酸和二乙烯基苯分别作为功能单体和交联剂,采用沉淀聚合法合成了甲苯分子印迹聚合物。静态平衡吸附实验结果表明,所得到的印迹聚合物对甲苯具有较强的选择性吸附能力,最大吸附容量为21.6 mg/g。将所制备的印迹材料作为固相萃取填料,对自来水样品中的甲苯进行选择性分离富集,加标回收率在92%~103%之间。     

槲皮素分子印迹聚合物合成及识别研究

以槲皮素(Quercetin)为模板分子,丙烯酰胺(AM)和4-乙烯基吡啶(4-VP)为双功能单体,三羟甲基丙烷三甲基丙烯酸酯(TRIM)为交联剂,采用沉淀聚合法制备槲皮素分子印迹聚合物(MIPs)并对其性能进行了考察。实验考察了致孔剂的体积、功能单体种类以及功能单体比例等因素对槲皮素MIPs吸附容量和选择性的影响。实验结果表明:以40 mL致孔剂、1:1AM/4-VP混合功能单体采用沉淀聚合法制备的MIPs吸附容量达到6.93μmol/g,是传统本体聚合法制备的MIPs吸附量的3.08倍,并且此法制备的MIPs相比本体聚合法具有更好的特异性识别能力和分离能力,分离因子α达到4.33;本文还将制备的MIPs用作固相萃取(SPE)吸附剂,优化了固相萃取的实验条件并采用SPE的方式对实际油茶壳样品中的槲皮素进行分离富集,试验结果表明用MIPs固相萃取处理后的油茶壳提取液中槲皮素的含量能达到83%,说明了槲皮素分子印迹固相萃取对实际油茶壳样品中槲皮素具有较好的分离、纯化效果。     

Research Progress of Sample Pretreatment of Phenolic Environmental Estrogens

酚类环境雌激素是最为常见的环境雌激素之一,其对人类、环境和生态的影响受到世界范围的关注.介绍了酚类环境雌激素的种类和毒性,详细讨论了各种样品前处理技术,包括溶剂萃取、索氏提取、固相萃取、基质固相分散萃取、微波辅助萃取、加速溶剂萃取、膜萃取、固相微萃取、搅拌棒吸附萃取、分子印迹聚合物萃取、超声辅助萃取、离子液体萃取、浊点萃取、超临界流体萃取等,并对酚类环境雌激素的样品前处理技术进行了总结和展望.     

加替沙星分子印迹聚合物的合成及应用研究

以加替沙星为模板分子,采用沉淀聚合的方法制备了分子印迹聚合物(MIPs),对制备条件进行选择,利用静态吸附实验研究了聚合物对目标分子及其结构类似物的识别特性。聚合物对加替沙星的最大吸附量为28.87 mg/g,对加替沙星具有良好的吸附性能。以该印迹聚合物微球为固相萃取材料填充固相萃取柱,结合高效液相色谱法测定加替沙星回收率达到92%~99%,富集倍数为213。与C18柱相比,制备的聚合物具有更好的选择性与富集倍数,可用于环境中加替沙星的富集与分离。     

基于改性花生壳的SPE-FAAS法测定环境废水中铬

采用化学方法制备了改性花生壳吸附材料,将其作为固相萃取剂建立了固相萃取-火焰原子吸收光谱(SPE-FAAS)测定环境废水中铬的方法。考察了样品pH、进样体积、流速、洗脱剂种类及共存离子等对萃取率的影响。评价了萃取材料的吸附容量及再生性能。在优化条件下,该法的检出限(3σ)为3.0 ng.mL-1,相对标准偏差(RSD)为3.8%(c=40 ng.mL-1,n=7),富集倍数为28.4倍。     

超临界流体萃取脱除人参中痕量有机氯农药

利用在线固相吸附柱收集,淋洗剂洗脱超临界流体萃取出的真实人参样品中的有机氯农残实验,确定最佳的吸附柱和淋洗剂。通过实验确定利用C18作吸附剂,用正己烷洗脱可取得最优效果。此外,还对直接冷凝收集法、索氏提取法与固相吸附柱收集法进行了对比。     

酚类环境雌激素的样品前处理技术研究进展

酚类环境雌激素是最为常见的环境雌激素之一,其对人类、环境和生态的影响受到世界范围的关注。介绍了酚类环境雌激素的种类和毒性,详细讨论了各种样品前处理技术,包括溶剂萃取、索氏提取、固相萃取、基质固相分散萃取、微波辅助萃取、加速溶剂萃取、膜萃取、固相微萃取、搅拌棒吸附萃取、分子印迹聚合物萃取、超声辅助萃取、离子液体萃取、浊点萃取、超临界流体萃取等,并对酚类环境雌激素的样品前处理技术进行了总结和展望。     

核壳型磁性表面分子印迹聚合物的制备及对罗丹明6G吸附性能研究

以罗丹明6G为模板分子,多巴胺和3-氨基苯硼酸为功能单体和交联剂,采用表面分子印迹技术,首次制备了对罗丹明6G具有优良吸附作用的核壳型磁性表面分子印迹聚合物。应用扫描电镜、透射电镜、红外光谱等对其进行表征,通过静态、动态和选择性吸附实验,研究了该分子印迹聚合物的识别选择性和吸附容量,并建立了固相萃取-分光光度法测定实际样品中痕量罗丹明6G的新方法,检测限为2.7nmol/L,回收率为86.9%~105.0%。     

糠醛分子印迹聚合物的制备及吸附性能研究

以糠醛为模板分子,采用本体聚合法制备了对糠醛具有高特异吸附性的糠醛分子印迹聚合物。利用扫描电镜和红外光谱对聚合物进行表征分析,并利用动态吸附、静态吸附和选择性吸附实验考察糠醛印迹聚合物的吸附性能。结果表明,所制备的糠醛分子印迹聚合物对糠醛呈现出较好的特异性吸附能力,有望作为固相萃取材料应用于食品中糠醛残留的分离、富集和检测。     

日用级三聚氰胺甲醛模塑料的制备

以三聚氰胺甲醛树脂为胶粘剂,纤维素为增强材料,制得三聚氰胺甲醛模塑料。通过测试模塑料的力学性能、流动性、挥发分及模收缩率和吸水率等,研究了三聚氰胺与甲醛配比、反应终点控制、纤维素含量、干燥温度、模塑粉细度等对模塑料性能的影响。结果表明,三聚氰胺与甲醛物质的量比为1∶2.5、终点控制在水浊度1∶3,纤维素用量42%~48%,干燥温度70℃,球磨至100~120目时,制得的模塑料性能良好,符合国家日用级产品相关标准。     

β-Cyclodextrin Based Molecularly Imprinted Solid Phase Extraction for Class Selective Extraction of Priority Phenols in Water Samples

Molecular imprinted polymer (MIP MAA-β-CD) with 2,4-dichlorophenol (2,4-DCP) and methacrylic acid functionalized β-cyclodextrin (MAA-β-CD) as the template molecule and the functional monomer, respectively, was prepared and used in molecular imprinted-solid phase extraction (MISPE) for the extraction of phenols (2,4-dichlorophenol, 2-chlorophenol, 4-chloro-3-methylphenol, 4-chlorophenol, 2,4,6-trichlorophenol, and 2-nitrophenol) from water samples. The MISPE method was optimized prior to the determination using gas chromatography coupled with a flame ionization detector (GC-FID). Under the optimized conditions, the MIP MAA-β-CD sorbent showed good linearity (0.01-12 mgL^?1), low limits of detection (0.14-0.75 µgL^?1), and good repeatability (RSD 2.3-3.6%, n = 3). Good recoveries were obtained in the range of 97-115% for tap water and between 88-103% for river water. The developed MIP MAA-β-CD SPE was then compared with other adsorbents. The unique properties of β-CD and presence of imprinted cavities explains the higher extraction recoveries obtained for phenols when using MIP MAA-β-CD SPE.     

Synthesis and Evaluation of a Molecularly Imprinted Polymer for Solid Phase Extraction of Ethopabate from Chicken Tissue

In this paper the development and evaluation of a molecularly imprinted polymer (MIP) for ethopabate is described. Ethopabate (ETP), 4-acetamido-2-ethoxybenzoic acid methyl ester, is one of the antibiotics which is used as coccidiostat in poultry feeds. In the present study, two widely used functional monomers, methacrylic acid (MAA) and 4-vinylpyridine (4-VP) were compared theoretically and experimentally as the candidates for MIP preparation. Hyperchem software was employed to estimate binding energies between ETP and functional monomers and batch rebinding experiments were performed to study the binding characteristics of the polymers. The results showed that MAA is a better functional monomer to prepare MIP. UV/Vis and NMR spectroscopy were used as two common tools to study the interactions between ETP and MAA in the pre-polymerization mixture. Liquid chromatography experiments showed that the prepared MIP has recognition capability toward ETP in comparison with other structurally related compounds. The ETP-imprinted polymer was further applied for selective solid phase extraction (SPE) of ETP from a chicken tissue sample. The extraction yield of ETP was found to be quantitative (87 ± 3%) and the LOD and LOQ based on 3 and 10 times of the noise of HPLC profile were 0.05 and 0.32 ng ml^?1, respectively. It was confirmed that the binding ability of the prepared MIP for ETP was essentially sufficient in the presence of other compounds coexisting in tissue sample. Therefore, as a selective and efficient solid phase material, ETP-imprinted polymer has a high potential application in the analysis of residues of this antibiotic in chicken tissue samples.     

茶叶中农药残留联苯菊酯的GC-ECD及GC-MS测定

建立了气相色谱(GC-ECD)及气相色谱-质谱(GC-MS)法对茶叶中的农药残留联苯菊酯的检测方法。经4∶1正己烷-丙酮混合溶液提取,活性碳、氟罗里硅双柱或氨基复合柱净化,氮吹浓缩同时用GC-ECD及GC-MS检测,联苯菊酯在0.02⁰.2mg/L范围内线性良好,r为0.999,回收率达到85.0%0.2mg/L范围内线性良好,r为0.999,回收率达到85.0%¹19.0%,相对标准偏差为2.1%119.0%,相对标准偏差为2.1%⁹.6%,定量检出限为0.01 mg/kg。该方法操作简单、快速、净化效果好、灵敏度高、检出限低、准确、对设备要求低、检测效果良好。     

Determination of trace macrolide antibiotics in milk with online solid‐phase extraction with an ionic‐liquid‐based monolithic column

An ionic liquid (IL)‐based monolithic poly(ionic liquid glycidylmethacrylate‐co‐ethylene glycol dimethacrylate) column was prepared via in situ free‐radical polymerization with 1‐vinyl‐3‐butylimidazolium chlorine as one of the comonomers. The obtained monolithic column was used as the sorbent of solid‐phase extraction (SPE) and coupled with high‐performance liquid chromatography for the simultaneous determination of the macrolide antibiotics roxithromycin (ROX) and acetylspiramycin (ACE) in processed pure milk. The monolithic column was characterized by Fourier transform infrared spectrometry, scanning electron microscopy, nitrogen absorption–desorption, mercury intrusion porosimetry, and thermogravimetric analysis. The results reveal that the monolithic column exhibited a high selectivity and good permeability to the macrolide antibiotics in milk. The optimized method offered excellent linearity with a linear regression coefficient greater than 0.998. The precisions for interday and intraday were both less than 7.7%. The accuracies expressed by the recoveries for ROX and ACE were in the ranges 92.5–103.8 and 93.0–107.6%, respectively. Compared to the previous methods, this method had a low limit of detection and a good accuracy. As a result, the polymer IL based monolithic column could feasibly be used as a high‐selectivity online SPE sorbent for determining trace macrolide antibiotics in milk. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43943.     

硅胶表面罗丹明B分子印迹聚合物的制备及其性能研究

以表面接枝乙烯基的硅胶为载体,罗丹明B为模板分子,丙烯酰胺为功能单体,乙二醇二甲基丙烯酸酯为交联剂,制备了表面印迹聚合物微球。通过静态吸附对吸附性能进行分析。结果表明,该印迹聚合物对模板分子具有特异吸附性能,并将其应用于固相萃取,测得罗丹明B的加标回收率为94.4%~101.2%,相对标准偏差(n=3)的范围为2.4%~3.4%。     

硅胶衍生尼古丁印迹整体柱的制备及其识别

采用原位聚合并表面接枝制备了硅胶衍生尼古丁印迹整体柱。红外光谱和扫描电镜研究了聚合物的结构,基于尺寸排阻色谱原理测定了整体柱的总孔和微孔体积。在高效液相色谱系统中,考察了色谱条件对整体柱选择性的影响;用前沿色谱法测试了MIP整体柱的等温吸附,并研究了整体柱的吸附热力学。结果表明： MIP整体柱对尼古丁的选择因子相对8-羟基喹啉和吡啶分别为4.31和2.95;当流动相中pH值为7.5时,选择性最好;Freundlich模型比Langmuir模型更适合描述尼古丁在印迹整体柱上表面位点分布,位点异化指数为0.841;吸附热力学分析表明尼古丁在印迹整体柱上的自发放热吸附过程。     

Synthesis and characterization of molecularly imprinted poly(methacrylic acid)/silica hybrid composite materials for selective recognition of lincomycin in aqueous media

A novel molecular imprinting method for the preparation of molecularly imprinted poly(methacrylic acid)/silica hybrid composite materials (MIP‐HCMs) for the selective recognition of lincomycin (LIN) in aqueous media by prepolymerization and free‐radical copolymerization was investigated. In this study, methacrylic acid was selected as the functional monomer, methacryloxypropyltrimethoxysilane was used as the crosslinker, and tetraethoxysilane was used as the inorganic precursor. MIP‐HCM was characterized by FTIR spectroscopy, the Brunauer–Emmett–Teller method, and TGA. The selectivity of the sorbent was investigated by a batch competitive binding experiment with an aqueous LIN and clindamycin (CLI) mixture. The selectivity coefficient for LIN in the presence of CLI was 6.27, whereas the relative selectivity coefficient between LIN and CLI was 5.83. The absorption capability of MIP‐HCM and the selectivity coefficient were much higher than those of the nonimprinted blank polymer. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2012     

柑橘中除草醚残留量的气相色谱-质谱法测定

建立了柑橘中除草醚除草剂农药残留量气相色谱质谱检测方法。用乙腈提取试样中残留的药物,经中性氧化铝固相萃取小柱净化,采用气相色谱分离,质量选择检测器检测,外标法定量。除草醚农药在0.01μg/mL～5.0μg/mL浓度范围具有良好线性关系,线性相关系数在0.9989～0.9996,空白样品中添加0.01 mg/kg、0.05 mg/kg、0.1 mg/kg三个浓度,回收率在80.1%～104.3%之间,相对标准偏差在3.2%～14.3%之间。以信噪比为10计的方法检测限(LOD)为0.01 mg/kg,方法快速、简单,完全能够满足农药残留检测要求。     

高效液相色谱测定环境水中2，4-二氯苯氧乙酸的方法研究

建立了以高效液相色谱法进行分离和检测环境水中2,4-二氯苯氧乙酸的方法。环境水中的2,4-二氯苯氧乙酸用SPE C18小柱进行固相萃取。液相色谱的条件是：色谱柱：SPE C18 150mm×4．6mm;流动相：甲醇：水（9：1,V／V）;流速：3mL·min^-1;柱温：40℃;检测器：UV 282nm;进样量10μL。回收率〉98％,最低检测限为0．01mg·L^-1。本法具有良好的灵敏度和重现性。