3D打印技术在有机合成化学中的应用

相对于传统的材料去除-切削加工技术,3D打印作为一种"自下而上"的材料累加制造方法,不仅操作简单、制造成本更低以及可实现快速生成,而且可实现复杂结构件的精确定制.因此,3D打印已成为第三次工业革命的代表性技术.近年来,化学家们将3D打印技术与有机合成相结合,在多通道异相催化剂和新型反应装置的研发设计等方面取得了积极的进展,进而使这项技术在有机合成领域中应用越来越广泛.对近年来基于3D打印技术的有机合成研究进展进行了综述,涵盖基于3D打印异相催化剂或催化剂载体、3D打印反应装置和3D打印流反应器,并对该领域的发展趋势进行了展望.     

微型气相色谱的研究进展

具有高性能、智能化、低功耗、低物耗的分析仪器微型化研究已经是分析仪器的主要发展方向。气相色谱(GC)作为一种应用十分广泛的分离分析仪器,其微型化的研究一直受到科学界和工业界的重视。本文综述了近十几年来微型气相色谱(micro GC)的研究进展。对微型气相色谱的3个主要组成部分,即进样/富集装置、色谱柱和检测器,分别进行了详细的阐述,并简单总结了微型气相色谱的应用现状,对其发展趋势进行了展望。     

通过一步萃取将组蛋白分为多个亚组分的蛋白质组预分离方法的建立

将基于正丙醇、氯化钠和水的双水相体系用于蛋白质组的预分离研究, 并考察了体系酸度及在不同浓度的盐、正丙醇及蛋白质存在时该双水相体系对蛋白质的分离效果. 将经该双水相体系预分离过的蛋白质组样品在未与成相试剂分离的条件下直接用于凝胶电泳分析. 结果表明, 该双水相体系可通过一步萃取将蛋白质组样品分为3个亚组群. 该蛋白质组预分离方法简单、快速、成本低, 并具有生物相容性、可连续操作性、无需昂贵复杂仪器以及在进行电泳分析前无须(或易于)将目标蛋白与成相试剂分离等优点. 该蛋白质组预分离方法的建立在蛋白质组学和方法学方面均有着极为重要的意义.     

微小型近红外光谱仪的应用进展与展望

近些年,近红外光谱分析技术得到了迅猛发展,该技术可直接对气体、液体和固体等各种复杂混合物进行定性和定量分析,具有分析速度快、效率高,可实现无损和在线分析等优势,在科研和工农业生产中发挥着越来越重要的作用。近红外光谱分析仪的微小型化是一个重要的发展方向,近期出现了众多不同类型的商品化微小型近红外光谱仪器。手持式或便携式现场快速分析是一种更经济、更高效、更灵活的方法,具有小体积、低功耗、低成本、便于二次开发等优点,在农业、食品、医药、石油化工和安全等众多领域获得了广泛的研究与应用。物联网技术在智能农业、智能工厂、智能医疗和智慧城市等众多领域的兴起,成为推动近红外光谱传感器向着微型化方向发展的主要力量。该文主要综述了近些年新型的商品化微小型（便携式、手持式和袖珍式）近红外光谱仪器及其应用进展,并对该技术的发展趋势和应用前景进行了展望。     

基于智能手机的便携式毛细管电泳装置检测消毒剂中2种季铵盐

现有的小型毛细管电泳(CE)装置仍采用平板或计算机进行数据处理和分析,其便携性仍存在明显不足。针对这一问题,发展了一种基于智能手机的CE装置,实现了真正的便携式定量分析。该装置集成了电容耦合式非接触式电导检测(C⁴D)和蓝牙通信功能,并提供了手机界面软件。通过手机界面软件,不仅可以控制CE装置的电泳运行,还可以实时接收C⁴D检测器发出的数据信息,显示电泳图谱和进行数据处理。该装置尺寸为20 cm×20 cm×15 cm,重量为2 kg。为了验证所设计装置的性能,采用季铵盐(QAs)消毒剂(十二烷基二甲基苄基溴化铵(DDBAB)和十二烷基三甲基溴化铵(DTAB))作为分析对象。实验数据表明,DDBAB和DTAB线性范围分别为20~1000和30~1000 μmol/L,线性回归方程的相关系数(R²)分别为0.9995和0.9989,检出限(LOD)分别为10和13 μmol/L,日内相对标准偏差(RSD, n=3)分别为1.9%和2.7%。另外实验对DDBAB和DTAB混合离子液进行了测试,在8 min内可实现基线分离。最后,对现场使用的新洁尔灭消毒液中QAs进行了加标回收试验,DDBAB和DTAB的回收率分别为100.5%~101.5%和96.2%~99.3%。研究结果表明,所开发CE装置具有线性好、LOD低、重复好、准确性高,尤其便携好等优点,可用于消毒液中QAs现场定量检测。     

微流控分析芯片发展与展望

1　引言　　当前许多发达国家已把现代科学仪器当做信息社会的源头和基础纳入未来发展的战略重点 ,而分析仪器又是其中最重要的组成部分之一。最近 ,人类基因组计划的提前完成充分说明了先进的分析仪器与技术在现代高科技发展中的重要甚至关键作用。面临着 2 1世纪科技发展中提出的众多挑战 ,分析仪器和分析科学也正经历着深刻的变革 ,其中一个日益明显的发展趋势就是化学分析设备的微型化、集成化与便携化。当前 ,分析仪器的发展正在出现一个以微型化为主要特征的、带有革命性的重要转折时期。在当前发展较快的微分析系统中 ,以 1 990年由…     

离子色谱法测定蔬菜硝酸盐含量

建立了化学抑制电导检测离子色谱法定性定量分析蔬菜硝酸盐含量的方法。阴离子分离柱DionexAS14柱(4mm×250mm),保护柱IonPacAG14(4mm×50mm)。流动相为1.7mmol.L-1NaHCO3,1.8mmol.L-1Na2CO3。流速1.2mL.min-1,自动连续再生抑制装置SRS-ULTRA4mm。线性范围为0.1~100.0mg.L-1,线性关系为0.9997,检出限为0.05mg.L-1。应用此法,测定了多种蔬菜硝酸盐含量。方法操作简单、快速、基体干扰少、灵敏、准确。     

双水相萃取-磁性阳离子交换剂联用分离蛋白质

双水相萃取(ATPS)分离蛋白质是基于蛋白质在上下两相间分配系数不同而达到彼此分离,它是一种简单、快速、低成本的蛋白质分离富集方法.表面修饰的磁性粒子与目标蛋白结合,在外加磁场作用下快速与原溶液分离,可实现目标蛋白分离和富集.双水相萃取与磁性分离均具有简单快速、条件温和的优点,在生物分离工程领域具有重要的应用价值.本文将双水相体系与热溶剂法制备的表面羧基功能化的磁性阳离子交换剂联用,用于蛋白质的逐级分离.     

微流控芯片简易安培检测器的制作及对烟酰胺片中烟酰胺的测定

搭建了微流控芯片简易安培检测器,并用于市售药品烟酰胺片中烟酰胺含量的测定。由碳纳米管微圆盘电极和钛管组成集成双电极,中间的碳纳米管微圆盘电极作为安培检测的工作电极,外套的钛管既作为安培检测的对极,又充当分离高压电源的地极,使其结构更加简化和微型化。优化了缓冲溶液种类、浓度,分离电压及进样时间等实验条件。结果表明,在10 mmol·L-1磷酸盐缓冲液(pH 7.8)中,进样10 s,在2.0kV电压下分离,烟酰胺在2 min内可实现较好的分离和检测,其线性范围为10~600μmol·L-1,检出限(S/N=3)为5.0μmol·L-1,相对标准偏差(RSD)为3.0%,平均加标回收率为99.1%。该装置实现了微型化和集成化,并具有检测灵敏度较高、选择性好、成本低等特点,可用于药品的质量控制。     

碳量子点荧光成像法应用于聚丙烯酰胺凝胶电泳检测人血清蛋白质的研究

建立了碳量子点荧光成像法检测聚丙烯酰胺凝胶电泳分离蛋白质如人血清蛋白质的新方法. 通过一步绿色微波法合成的碳量子点并将其应用在聚丙烯酰胺凝胶电泳分离蛋白质的检测中, 通过醋酸-醋酸钠调节孵育溶液, 优化pH值、碳量子点的用量及孵育溶液的浓度等条件, 使碳量子点和蛋白质相结合并在365 nm的紫外灯照射下得到了清晰的人血清蛋白电泳图, 该新方法具有原料便宜易得、无污染、简单、快速、高灵敏度、低背景及高分辨率的优点, 在生物技术方面和纳米技术方面具有巨大的应用前景.     

Miniaturization of Slab Gel Electrophoresis Using Thermal Lens Microscope and its Application to Genetic Diagnostics

Slab gel electrophoresis is the most widely used separation method for DNA fragments, proteins and carbohydrates, and miniaturization of this process is expected to provide fast, inexpensive and convenient analyses. However, two problems concerning the miniaturization of gel electrophoresis have to be solved:the separation performance and spatial resolution of the detector. We demonstrated that the separation performance was improved by using a discontinuous gel in which a concentrating gel was used to stack the sample to a sharp band, and using thermal lens microscope (TLM), which is highly sensitive and has a spatial resolution of micron level even in light scattering matrices as a gel, such sharpened separated bands were successfully detected. In this paper, we developed a miniaturized slab gel electrophoresis apparatus, demonstrated high speed separation of DNA fragments, and applied it to genetic diagnosis of coronary heart disease.     

Integration of isoelectric focusing with multi-channel gel electrophoresis by using microfluidic pseudo-valves

Two-dimensional (2D) protein separation is achieved in a plastic microfluidic device by integrating isoelectric focusing (IEF) with multi-channel polyacrylamide gel electrophoresis (PAGE). IEF (the first dimension) is carried out in a 15 mm-long channel while PAGE (the second dimension) is in 29 parallel channels of 65 mm length that are orthogonal to the IEF channel. An array of microfluidic pseudo-valves is created for introducing different separation media, without cross-contamination, in both dimensions; it also allows transfer of proteins from the first to the second dimension. Fabrication of pseudo-valves is achieved by photo-initiated, in situ gel polymerization; acrylamide and methylenebisacrylamide monomers are polymerized only in the PAGE channels whereas polymerization does not take place in the IEF channel where a mask is placed to block the UV light. IEF separation medium, carrier ampholytes, can then be introduced into the IEF channel. The presence of gel pseudo-valves does not affect the performance of IEF or PAGE when they are investigated separately. Detection in the device is achieved by using a laser induced fluorescence imaging system. Four fluorescently-labeled proteins with either similar pI values or close molecular weight are well separated, demonstrating the potential of the 2D electrophoresis device. The total separation time is less than 10 minutes for IEF and PAGE, an improvement of 2 orders of magnitude over the conventional 2D slab gel electrophoresis.     

Sodium dodecyl sulfate free gel electrophoresis/electroelution sorting for peptide fractionation

Shotgun proteomics based on peptide fractionation by using liquid chromatography has become the common procedure for proteomic studies, although in the very beginning of the field, protein separation by using electrophoresis was the main tool. Nonetheless, during the last two decades, the electrophoretic techniques for peptide mixtures fractionation have evolved as a result of relevant technological improvements. We also proposed the combination of sodium dodecyl sulfate polyacrylamide gel electrophoresis for protein fractionation and sodium dodecyl sulfate free polyacrylamide gel electrophoresis for peptide separation as a novel procedure for proteomic studies. Here, we present an optimized device for sodium dodecyl sulfate free polyacrylamide gel electrophoresis improving peptide recoveries respect to the established electrophoretic technique off gel electrophoresis meanwhile conserving the excellent resolution described for the former technique in slab gel based systems. The device simultaneously allows the separation and the collection of fractionated peptides in solution.     

A novel method that improves sensitivity of protein detection in PAGE and Western blot

We have developed a simple and inexpensive method that improves sensitivity of protein and antigen detection in standard PAGE procedures. Our technique uses a sample microloader device with a funnel‐like structure, filled with a 4% stacking gel. When attach to the top of a polyacrylamide slab gel, the proteins in a sample are concentrated by electrophoresis into a small volume as they emerge from the device's narrow outlet. Our microloader has several advantages over previous devices, including simple assembly, high versatility, and absence of cross‐contamination between lanes. Addition of this device to a slab gel results in a fivefold increase in the sensitivity of antigen detection in a Western blot. As a result, less protein is required for loading and signal detection. Our protocol is a straightforward modification of a standard experimental technique, and is especially useful when only limited sample quantities are available.     

Comparative study between a commercial and a homemade capillary electrophoresis instrument for the simultaneous determination of aminated compounds by induced fluorescence detection

The performance of two capillary electrophoresis (CE) instruments, one commercial and one homemade device, were compared for the determination of derivatised aminated compounds with fluorescein isothiocyanate (FITC). The commercial CE system first uses an argon ion laser as excitation source; the homemade CE device uses an inexpensive blue-light-emitting diode (LED) as the light source and a charge-coupled device (CCD) as the detection system. After fine optimisation of several separation parameters in both devices, a co-electroosmotic flow CE methodology was achieved in coated capillary tubing with 0.001% hexadimetrine bromide (HDB), and 50 mmol L⁻¹ sodium borate at pH 9.3 with 20% 2-propanol for the determination of several amines and aminoacids. Analytical performances, applicability in beer samples and other aspects such as cost or potential for miniaturization have been compared for both devices.     

High-performance ultrathin layer agarose gel electrophoresis

Large scale, high-resolution DNA fragment analysis, such as genotyping, mapping and genetic profiling requires an affordable, fully automated high-throughput gel electrophoresis based separation device that enables rapid, high-performance analysis in a wide molecular weight range. In this article a novel approach is described that greatly enhances the productivity of DNA fragment analysis by automating the current manual procedure and also reducing the separation time and human intervention from sample loading to data analysis. The ultrathin layer, multilane, high-performance agarose gel electrophoresis system employs integrated scanning laser induced fluorescence-avalanche photodiode detection and combines the advantages of conventional slab and capillary gel electrophoresis. The separation platform is fabricated in a way that the sieving matrix can be easily replaced in the separation cassette for each run. Visualization of the DNA fragments is accomplished by ‘in migratio' complexation during the electrophoresis process with ultra-sensitive fluorescent agents, also enabling real-time imaging and data analysis.     

Protein identification from two-dimensional gel electrophoresis by connecting ZipTip with a home-assembled nanoflow system

Mass spectrometry (MS) is a powerful technique for protein identification in proteomic research. Two-dimensional gel electrophoresis (2-DE) combined with MS is a significant method for protein separation and identification. For protein identification, peptide sequencing is usually carried out by an effective but expensive nano-flow liquid chromatographic system combined to tandem mass spectrometry (MS/MS). However, protein identification based on such method is time-consuming, and contamination may occur as a result of column overloading. In this study, we establish an alternative nanoscale system for protein identification using MS/MS. The system consists of several devices that can be purchased from commercial sources and can be connected to an electrospray ionization quadrupole-time of flight (ESI-Q-TOF) MS in order to analyze proteins from 2D gels. This inexpensive strategy provides an attractive alternative method for rapid identification of proteins using a nanospray source. In addition, the device is disposable so that contamination is avoided. It is shown that peptide sequencing based on this device using ESI-Q-TOF MS is accomplished within 10 min.     

Material and structural design of microsupercapacitors

Journal of Solid State Electrochemistry - With the rapid development of miniaturization and miniaturization of portable electronic devices, the requirements of electronic devices are increasing for...     

Parallel processing in the isoelectric focusing chip

Investigation of isoelectric focusing (IEF) kinetics has been performed to provide the theoretical basis for miniaturization of classical IEF in immobilized pH-gradients. Standard IEF demands colinearity of the electric field and pH-gradient directions (serial devices). It is shown that the IEF separation process based on a continuous, serial pH gradient is incompatible with miniaturization of separation devices. The new realization of the IEF device by a parallel IEF chip is suggested and analyzed. The main separation tool of the device is a dielectric membrane (chip) with conducting channels that are filled by Immobiline gels of varying pH. The membrane is held perpendicular to the applied electric field and proteins are collected (trapped) in the channels whose pH are equal to the pI of the proteins. The pH value of the surrounded aqueous solution is not equal to any channel's pH. The fast particle transport between different channels takes place due to convection in the aqueous solution. The new device geometry introduces two new spatial scales to be considered: the scale of transition region from a solution to the gel in a channel and a typical channel size. The corresponding time scales defining the IEF process kinetics are analyzed and scaling laws are obtained. It is shown both theoretically and experimentally that parallel IEF accelerates the fractionation of proteins by their pI down to several minutes and enables possible efficient sample collection and purification.     

Miniaturized free-flow electrophoresis: production,optimization, and application using 3D printing technology

The increasing resolution of three-dimensional (3D) printing offers simplified access to, and development of, microfluidic devices with complex 3D structures. Therefore, this technology is increasingly used for rapid prototyping in laboratories and industry. Microfluidic free flow electrophoresis (μFFE) is a versatile tool to separate and concentrate different samples (such as DNA, proteins, and cells) to different outlets in a time range measured in mere tens of seconds and offers great potential for use in downstream processing, for example. However, the production of μFFE devices is usually rather elaborate. Many designs are based on chemical pretreatment or manual alignment for the setup. Especially for the separation chamber of a μFFE device, this is a crucial step which should be automatized. We have developed a smart 3D design of a μFFE to pave the way for a simpler production. This study presents (1) a robust and reproducible way to build up critical parts of a μFFE device based on high-resolution MultiJet 3D printing; (2) a simplified insertion of commercial polycarbonate membranes to segregate separation and electrode chambers; and (3) integrated, 3D-printed wells that enable a defined sample fractionation (chip-to-world interface). In proof of concept experiments both a mixture of fluorescence dyes and a mixture of amino acids were successfully separated in our 3D-printed μFFE device.