芯片毛细管电泳荧光检测器灵敏度的研究

本文采用倒置荧光显微镜,以汞灯为激发光源,自行设计组装了芯片毛细管电泳荧光检测系统。以荧光素异硫氰酸酯(FITC)为检测对象,对双通道门控光子计数器、CH151型光子计数探测器、电荷耦合器件(CCD)三种荧光检测器的灵敏度进行了比较研究。根据芯片毛细管电泳图谱分析,FITC在双通道门控光子计数器、CH151型光子计数探测器、CCD三种检测器中的检出限(S/N=3)分别为7.0×10-10mol/L,1.2×10-9mol/L,3.2×10-8mol/L。进一步采用CH151型光子计数探测器和CCD两种较常用检测器,对FITC和荧光素、曙红和荧光素两组荧光试剂的分离及检测进行了研究。结果表明,使用CH151型光子计数探测器作为检测器,灵敏度高,基线稳定,信噪比高。     

汞灯光源芯片毛细管电泳荧光电荷耦合器件检测系统

以宽谱带高压汞灯为光源的倒置荧光显微镜,配备电荷耦合器件(CCD)及微流控芯片,自组装芯片毛细管电泳荧光电荷耦合器件检测系统。选择不同激发波长(340~540 nm)荧光试剂,进行荧光检测,荧光素的检出限(S/N=3)为7.3×10-9mol/L,荧光素异硫氰酸酯(FITC)的检出限(S/N=3)为1.7×10-8mol/L,显示了该系统对荧光试剂选择范围宽、灵敏度高的特点。用该系统成功分离了FITC与荧光素、曙红与荧光素两种混合荧光试剂。实验表明,组装的芯片毛细管电泳CCD荧光检测系统是成功的。     

二维毛细管电泳电化学检测尿样中的β-阻断剂

设计并制作了在柱电化学(EC)检测池,用于在同一根毛细管中进行中心切割二维毛细管电泳(2D-CE)在线纯化分离检测尿样中的6种β-阻断剂.尿样先在15 mmol/L NaAc缓冲液中进行毛细管区带电泳(CZE)分离,带正电荷的β-阻断剂与中性和带负电荷的干扰物质分成不同区带,然后在检测端施加13.8 kPa压力将干扰成分从毛细管入口端排出,同时将目标组分驱送到毛细管入口端,最后在90 mmol/L NaAc-30 mmol/L SDS缓冲液中进行胶束电动毛细管色谱(MEKC)分离.场放大样品堆积(FASS)/胶束推扫在柱双重富集技术不仅有效抵消压力驱送过程中产生的区带扩散,还可进一步压缩样品区带,提高检测灵敏度.本方法成功用于服药后鼠尿样品中6种β-阻断剂的分离测定,经第一维CZE分离排除干扰后,在未涂层毛细管柱(60 cm ×50 μm i.d.)、90 mmol/L NaAc/HAc-30 mmol/L SDS运行缓冲液、检测电位0.8 V、运行电压10 kV条件下,对6种β-阻断剂进行在线富集分离,峰高、峰面积和迁移时间的相对标准偏差(RSD)分别为2.0%～4.1%, 1.4%～3.7%和0.9%～2.7%(n=6).本研究为毛细管电泳在复杂样品在线纯化分析等方面的应用提供了新方法.     

免疫亲和毛细管电泳的研究进展

免疫亲和毛细管电泳方法结合了免疫分析的高特异性和毛细管电泳分离的高效、快速、样品用量少等优点,是复杂样品中特定组分分析的重要方法之一。激光诱导荧光检测器的使用以及毛细管电泳分离前免疫预富集过程的引入,可以进一步提高分析测定的灵敏度,使其能够用于痕量物质的高灵敏测定。本文结合作者所在课题组的工作,对免疫亲和毛细管电泳的两种主要模式,即均相的毛细管电泳免疫分析(CEIA)和非均相的免疫亲和毛细管电泳(IACE)的研究进展进行了综述。     

CZE-ESI-MS联用测定小肽混合物的研究

研究肽的分离行为、测定方法及测定条件对蛋白质组学研究具有重要意义 .毛细管电泳 ( CE)作为一种高效、快速的分离方法 ,样品用量少 ,已被广泛应用于生物领域中 ,尤其是小肽和蛋白质的分离分析 .质谱 ( MS)能够进行微量鉴定 ,并提供精确的分子量和结构信息 ,使其成为小肽和蛋白质检测和序列测定的强有力的支撑技术之一 [1～ 3] .其中 ,电喷雾 ( ESI)质谱作为一种软电离技术 ,易与常规的高分辨率分离方法如高效液相色谱、毛细管电泳等实现在线联用 ,具有分离效率高、检测灵敏度高和样品定性方便等特点 ,因而在小肽和蛋白质的测定中得到广…     

毛细管电泳和毛细管电色谱技术在农药残留检测中的应用

由于毛细管电泳（CE）和毛细管电色谱（CEC）具有所需样品体积小、分离效率高等特点,越来越多的学者已将它们应用到农药残留（简称农残）检测中,并将它们同各种不同的检测器以及样品浓缩方法相结合,以提高检测的灵敏度。本文对CE和CEC两种方法中所涉及的常见的样品预浓缩方法进行了简要的介绍。对各种不同类型的检测器（如紫外检测、荧光检测、电化学检测以及质谱检测等）的优缺点及其在农残检测中的应用情况进行了评述;同时对手性农药的CE和CEC分离检测情况进行了特别介绍;并对CE和CEC在农残分析与检测中的应用前景进行了展望。     

一种便携式毛细管电泳-激光诱导荧光检测仪的研制及性能考察

正毛细管电泳技术(CE)自1981年提出以来,得到了快速的发展。由于采用高电场,其柱效高、分离速度快、样品用量少,在生命科学、环境检测、药物分析和食品检验等领域得到了广泛应用[1-4],其常见的检测方法有紫外-可见吸收法、化学发光法、电化学法及荧光法等[5]。在实际样品检测中,目标物的含量较低,且其检测信号还易受成分复杂的样品基质的干扰,因此,需要灵敏度高的分析方法。激光诱导荧光检测法是一     

毛细管电泳与化学发光检测联用方法的研究进展

毛细管电泳由于其超高的分离效率广泛应用于生物医药、环境监测、食品科学以及公共安全等领域。然而,由于毛细管电泳具有进样量较少、检测光程较短等缺点,需要与高灵敏度检测器联用实现低浓度样品的分析。化学发光检测由于其背景信号低而具有超高的灵敏度。毛细管电泳-化学发光检测联用方法将毛细管电泳的高效分离特性与化学发光检测的高灵敏性相结合,成为一种非常重要的分析方法,广泛用于化学分析、药物筛选以及环境监测等领域。该文对近年来毛细管电泳-化学发光检测联用方法的基本原理进行概述,并对其发展趋势和应用前景进行了展望。     

唾液中苯丙胺类毒品的毛细管区带电泳在线富集检测

采用毛细管区带电泳(CZE)中的场放大样品堆积(FASS)技术对唾液中的苯丙胺类毒品进行了检测.采用含30%(体积分数)甲醇的100mmol/L磷酸盐(pH3.0)为分离缓冲液,用水溶解样品,利用缓冲体系与样品溶液体系电导率的差异,在毛细管中浓缩样品组分,对苯丙胺(AM)、甲基苯丙胺(MAM)、3,4-(亚甲二氧基)苯丙胺(MDA)、3,4-(亚甲二氧基)甲基苯丙胺(MDMA)4种毒品进行了分离和定量测定.采用利多卡因为内标,对添加上述4种毒品的唾液进行液液提取并进行FASS-CZE检测,可检测到的上述毒品质量浓度为0.002mg/L,与常规毛细管区带电泳比较,灵敏度提高上千倍;相对标准偏差在1.4%～7.7%之间,回收率在74%～108%.该方法可用于生物检材中苯丙胺类毒品的检测.     

亲水作用加压毛细管电色谱-激光诱导荧光检测法分析痕量核黄素类物质

一种新型的亲水作用毛细管电色谱(HI-CEC)整体柱被应用于加压毛细管电色谱-激光诱导荧光检测(pCEC-LIF)联用法对核黄素类物质的分离分析。采用自组装的pCEC-LIF系统,实现了对痕量核黄素(RF)、黄素单核苷酸(FMN)和黄素腺嘌呤二核苷酸(FAD)的快速分析。在最优的分离检测条件下,3种化合物在8.0 min内完全分离,RF、FMN和FAD的检出限(LOD, S/N=3)分别为5.0×10－11 mol/L、8.0×10－10mol/L和2.5×10－9mol/L,测定线性范围可达3个数量级,精密度良好。方法简便、全分析时间短、灵敏度和选择性高,血清样品分析实验结果良好,可望进一步应用于体液及细胞中核黄素类物质的痕量检测     

Simultane instrumentelle Multielementbestimmung in antiker Keramik (Terra Sigillata) durch Aktivierungsanalyse mit hochenergetischen Photonen

A large number of fragments of ancient roman pottery has been analyzed for main constituents, minor and trace-elements using high-energetic photon activation analysis followed by high resolution gamma spectroscopy. Especially the environmental influence on the concentrations of the minor constituents and trace elements during deposition of the sherds in the soil has been examined. Finally, a comparison has been made between analysis data of ancient pottery obtained by photon activation analysis, X-ray fluorescence analysis and 14 MeV-neutron activation analysis.      

药物发光分析的研究与展望

本文概述了国内目前药物发光分析的现状着重对荧光，化学发光和磷光光谱法在药物分析中的应用作了较详细的介绍，此外还介绍了作者近几年来用发光技术与薄层分离联用进行药物含量测定，中药微量元素测定，血药浓度监测和药代动力学研究的研究工作，提出了药物发光分析研究了目前主要是要把高分离度与高灵敏度检测相结合及连续操作。     

甲醛监测方法及仪器

介绍了甲醛检测方法的新进展和常用的仪器,指出发展灵敏度高、选择性好、能够实现现场分析或长期稳定地实时在线监测的新方法和新仪器仍然是空气中甲醛监测研究的一个重要方向。     

Preparation and characterization of poly(copper 2,3,9,10,16,17,23,24-octacyanophthalocyanine)

Dark blue poly(copper 2,3,9,10,16,17,23,24-octacyanophthalocyanine) has been prepared by reacting 1,2,4,5-tetracyanobenzene with cuprous chloride in 1-methyl-2-pyrrolidone at ca. 150°C. The product has been characterized by elemental analysis, thermal analysis, infrared and UV-VIS spectroscopies. The polymer has high purity and exhibits good thermal stability in an inert atmosphere.     

基于微流控芯片的微阵列分析

微阵列芯片具有高通量、微量化和自动化等特点,已经在很多领域得到广泛应用。但是微阵列芯片仍然具有不足之处,如所需设备昂贵、分析时间较长、灵敏度不高、多样品平行分析能力不足等。微流控芯片微米级的通道具有相对较大的比表面积和较短的扩散距离,能够显著加快分析速度、提高检测效率、增强分析性能,并且能够加工大量的平行通道用于多样品分析。目前已经有大量文献报道将微流控芯片和微阵列芯片相结合,发展了独特的杂交方式并在实验和理论上分别证明了两者相结合的优势,本文综述了将微流控芯片技术应用于微阵列分析的研究进展,着重介绍了在微流控芯片上进行微阵列分析时的杂交方式、促进杂交的措施以及杂交过程的数学建模,同时也介绍了其他分析步骤方面的进展。最后分析了目前微流控芯片技术在进行微阵列杂交应用方面的不足及其原因,并指出这两项技术相结合的优势和未来。     

Chromatographic methods for petroleum fractions analysis

The state-of-the-art problem of the analysis of various petroleum fractions by the methods of high performance liquid and capillary gas chromatography, IR-spectroscopy, and mass-spectrometry has been considered. The core principle of high performance liquid chromatography as the principal method for petroleum fractions’ separation has been described. Some methods for the chemical modification of domestic silica have been presented. Methods for aromatic hydrocarbons in benzine, kerosene, and diesel petroleum fractions by the chromatography method have been described.     

Microanalysis of solid surfaces by Secondary Neutral Mass Spectrometry

Summary The application of Secondary Neutral Mass Spectrometry (SNMS) for high resolution microanalysis of solid surfaces is a rapidly evolving field. Significant progress which has recently been made, as the different SNMS techniques are further developed, includes two important aspects. First the outstanding capability of SNMS for depth profiling with high depth resolution, which in the past was essentially restricted to electrically conducting samples, has been extended towards the analysis of insulating materials with dielectric constants approaching unity. Second, great effort has been made to develop a secondary neutral microprobe which allows SNMS surface and in-depth analysis with high lateral resolution. Here two promising approaches exist, which are based on different methods for post-ionization of sputtered neutral particles. The present state-of-the-art of both techniques is shown and a comparison in respect to detection limits and image acquisition times is attempted.     

Protection of Copper Surface Against Corrosion by Cationic Surfactant in Seawater

The protection power of the cationic surfactant decylammonium acetate (DAA) in seawater has been studied to define the perfect conditions have to be found for using it as a corrosion inhibitor for copper surface. The adsorption isotherm of this surfactant on copper surface has been determined at different interval times at 30°C. The given isotherms have, in general, similar shapes exhibiting a Languimirian L-shape. The corrosion measurement has been determined according to weight loss method. The study declines that cationic DAA, in seawater, protects well the copper surface against corrosion when added with low concentrations, while high concentrations show bad inhibition efficiency. ICP spectroscopic analysis assures this result where high Cu% has been obtained in the presence of high DAA concentration.     

Aldehyde analysis by high performance liquid chromatography/tandem mass spectrometry

This paper describes the development of a high performance liquid chromatography/tandem mass spectrometric (MS/MS) procedure for the specific qualitative and quantitative analysis of lipid aldehydes in biological matrices. A derivatisation method, which results in molecules that exhibit a common product ion on MS/MS, permits informative precursor ion scans, at high sensitivity. This has been applied to the examination of plasma in order to examine the production of aldehydes consequent on in vitro lipid oxidation. Quantitative analysis of target molecules using multiple reaction monitoring has been developed to permit quantitation in the same matrices.     

Interfacial-chemistry mediated behavior of colloidal talc dispersions

Interfacial chemistry and rheological behavior of talc suspensions as a function of pH, talc solid content, and type and concentration of ions have been investigated using electrokinetic measurements, rheology, settling behavior, and solution analysis. Zeta potential measurements show a strong dependence on the pH history of the talc suspension that only occurs when the surface area (solid content) of the talc is high. Particle interactions measured through dispersion yield stress measurements show a similar dependence. Talc is a magnesium silicate mineral and the dependence seen in the electrokinetic properties in this study has been attributed to Mg(II) dissolution at low pH, and has been confirmed by solution analysis. At high solid content (>20 wt%), pronounced Mg(II) ion dissolution occurs at low pH values. Formation and adsorption of electropositive Mg(II) hydrolysis products occurs at high pH (>9), and these lead to zeta potential reduction and, at high solid contents, charge reversal. Particle interactions reflect the surface chemistry behavior. Consequently, for a freshly prepared suspension at high pH, the yield stress is lower compared to after the pH has been taken to 5 and subsequently increased.