Study on the Recognition of Azo Dye and Protein Moleculer by Molecularly Imprinted Technique

分子印迹技术是制备对特定分子具有专一识别性能的聚合物的技术，分子印迹聚合物对模板分子的识别具有预定性、专一性和实用性等优点而在生物模拟、分离提纯、免疫测定以及痕量分析等领域显示出广阔的应用前景。 本文对分子印迹技术，特别是生物大分子的印迹技术进行了一些研究和探讨，总共分为四个章节。 第一章，文献综述；对分子印迹技术的基本原理、分子印迹聚合物的制备和应用进行了总述，对分子印迹技术当前存在的问题和未来的发展趋势进行了分析和展望。 第二章，以α-甲基丙烯酸为功能单体，在氯仿溶剂中，利用传统的分子印迹聚合物制备技术，合成了偶氮类分子1-(2-吡啶偶氮)-2-萘酚的印迹聚合物。通过红外和紫外光谱等...Molecularly imprinted technique (MIT) is a new method that contains tailor-made recognition sides for certain molecules. It is with many characteristics such as pre-determinative, specific and practical abilities of molecule recognition. It has been extensively applied in biomimics, purification, separation and enrichment fields. In this dissertation, MIT, mainly including the protein template im...学位：理学硕士院系专业：化学化工学院化学系_分析化学学号：X20032500

Simultaneous Determination of Residues of Organochlorine and Pyrethroid Pesticides in Tea by Microwave Assisted Extraction Solid Phase Microextraction-Gas Chromatography

建立了微波辅助萃取-固相微萃取-气相色谱(MAE-SPME-GC)同时测定茶叶中六六六(α-BHC,β-BHC,γ-BHC,δ-BHC 4种异构体)、滴滴涕类(DDD,DDE,o,p′-DDT,p,p′-DDT)、氯氰菊酯(cypermethrin)和氰戊菊酯(fen-valerate)等10种农药残留的方法。采用外标法定量,除氰戊菊酯外,农药的质量浓度与其色谱峰面积在一定范围内有较好的线性关系,相关系数为0.970 5~0.998 4。10种组分的加标回收率为64%~121%,相对标准偏差为10.4%~22.9%,检测限为1~50 ng/L。应用该方法测定了市场上3种茶叶中上述农药残留的含量。The issue of residues including organochlorine and pyrethroid pesticides in tea has made a great attention of researchers and customers in the world.Although some analytical methods have well been established to detect these pesticides,the sample preparations are generally laborious,time-consuming,and some of the procedures caused environmental pollution.Solid phase microextraction(SPME) is a novel sample preparation technique since it is of simplicity,high efficiency and solvent free.SPME was firstly developed to address the need to facilitate environment monitoring.In recent years,great efforts have been made in the analysis of pesticide residues in agricultural products by SPME.In this research,a microwave assisted extraction solid phase microextraction-gas chromatography(MAE-SPME-GC) was applied for the simultaneous determination of organochlorine and pyrethroid pesticides,such as benzene hexa chlorides(α-BHC,β-BHC,γ-BHC and δ-BHC),1-(2-chlorophenyl)-1-(4-chlorophenyl)-2,2,2-trichloroethane(o,p′-DDT),2,2-bis(4-chlorophenyl)-1,1-dichloroethylene(DDE),2,2-bis(4-chlorophenyl)-1,1-dichloroethane(DDD),2-(2-chlorophenyl)-2-(4-chlorophenyl)-1,1,1-trichloroethane(p,p′-DDT),cypermethrin and fenvalerate.All the tested pesticides were baseline separated under the experimental conditions,except for DDD and o,p′-DDT.The concentration of each pesticide was calibrated by external standard method.The linearities were found to be in the correlation coefficient range of 0.9705 to 0.9984 for the tested pesticides between the mass concentrations and peak areas,except for fenvalerate.The recoveries,relative standard deviations and detection limits for the 10 pesticides were 64%-121%,10.4%-(22.9%,) and 1-50 ng/L,respectively.The proposed method was successfully applied to the determination of organochlorine pesticide residues in three kinds of teas from the local market.The experimental results demonstrated that MAE-SPME-GC was a fast,sensitive and green technique for the analysis of trace quantity of pesticides in solid substrate foods.福建省科技计划项目(2005I-030,2006Y0026

Study of Preparation and Binding Characteristics of Molecularly Imprinted Polymers for 1-(2-Pyridylazo)-2-naphthol

以α-甲基丙烯酸为功能单体,在氯仿溶剂中,利用传统的分子印迹聚合物制备技术,成功合成了偶氮类分子1-(2-吡啶偶氮)-2-萘酚的印迹聚合物。用红外光谱、紫外光谱等技术对聚合物进行了表征测定,并用平衡结合实验研究了聚合物的吸附特性。A molecularly imprinted polymer,1-(2-pyridylazo)-2naphthol,was synthesized with α-acrylic acid as a functional monomer in the chloroform solvent by classical molecularly imprinted technique.The polymer was characterized by IR,UV spectra and the equilibrium binding experiment.The adsorption capability and adsorption kinetics of the polymer was investigated in the study.The results showed that the molecularly imprinted polymer is highly selective to 1-(2-pyridylazo)-2-naphthol.福建省教育厅科技项目(No.JA07156

Rapid determination of dicofol in Chinese teas by GC/ECD using microwave-assisted extraction associated with solid phase microextraction

建立了微波辅助萃取-固相微萃取-气相色谱/电子捕获检测法快速测定茶叶中三氯杀螨醇的方法。采用自制的PDMS萃取头,优化了萃取溶剂的种类,微波辐射时间和微波功率等微波辅助萃取条件;研究了SPME萃取时间、搅拌速度、离子强度、解吸温度和解吸时间对萃取效率的影响。方法对三氯杀螨醇的检出限为0.048 ng/mL,线性范围为0.2~200 ng/mL。在优化的实验条件下,对乌龙茶进行添加回收试验,平均回收率为61.3%~72.8%,相对标准偏差为8.0%~16.3%。本方法适合于茶叶中痕量三氯杀螨醇快速检测。A microwave-assisted extraction(MAE) associated with solid phase microextraction(SPME) followed by gas chromatography-electron capture detector(GC-ECD) was developed for the determination of dicofol in tea samples.We used the homemade PDMS fiber as the SPME material in the experiment.The MAE conditions,such as the extraction type,irradiation time and irradiation power were optimized.Several factors influencing the SPME extraction efficiency such as extraction time,stir speed,ionic strength,desorption temperature and desorption time were investigated.The linear range of the method was from 0.2 to 200 ng/mL,and the detection limit was 0.048 ng/mL.Spiked tea samples were analyzed under the optimum MAE and SPME conditions.Recoveries of this method were between 61.3% and 72.8%,and the repeatability was found to be 8.0%～16.3%.The processed approach provides a simple and sensitive method for the rapid determination of dicofol in tea samples.福建省科技重点(2005I-030,2006Y005)项目资

Determination of organochlorine and pyrethroid pesticides in vegetable samples by ultrasonic extraction and SPME-GC method

建立了一种USE-SPME-GC联用测定蔬菜中有机氯和菊酯类农药残留量的新方法,并对分析条件进行优化和探讨,实验表明,萃取液中基体杂质和色素对分析结果干扰较大,我们提出稀释的方法较好的解决这个问题。对实际蔬菜样品进行了测定和分析。A new method used for the determination of organochlorine and pyrethroid pesticides from vegetable samples coupling ultrasonic extraction with SPME-GC is presented here.The experimental conditions were also controlled and optimised.It is showed that the residues and pigments,who can effect greatly the experimental results,were avoided by dilution.We also demonstrated the practical applicability of this method.福建省科技计划(2005I-030,2006Y0026);; 福建省教育厅科技(JA07156)项目资