Graded Materials of (TiB_2)_pNi with Nickel Substrate Prepared by Field-Activated Pressure-Assisted Synthesis Process

The preparation of functionally graded materials （FGMs） of （TiB2）pNi with an intermetallic compound media layer of Ni3Al and a substrate of nickel by field-activated pressure-assisted synthesis process （FAPAS） was investigated. Ni3Al was chosen as a layer of FGM for the first time due to its great deal of heat released during its synthesis from nickel and aluminium powder. The microstructure, phase composition of layers, micro-hardness and elemental concentration profiles across interfaces were characterized. The significant inter-diffusion of elements between layers showed the formation of good bonds. The measured micro-hardness values of the sample increased monotonically to more than 3 500 HK over a distance of 2 mm from the nickel substrate to the surface layer （TiB2）pNi. The results of this investigation demonstrate the feasibility of the FAPAS process for rapid formation of FGMs with good diffusion bonds.

Capillary Electrochromatography Using C_8 Open Tubular Column Prepared by Sol-Gel Technique

Open tubthar C8 columns were prepared by sol-gel technology and used in the electrochromatographic separations.

Separation of Peptides by Pressurized Capillary Electrochromatography

A novel gradient pressurized capillary electrochromatography (pCEC) instrument was developed to separate peptides. Two gradient elution modes, hydrophobic and hydrophilic interaction mode in pCEC, were performed on this instrument. Baseline separation of six peptides was obtained on two gradient modes with C18 column and strong cationic exchange column respectively. The effects of mixer volume and total flow rate of pumps on resolution were also discussed.

Rapid Preparation of Monolithic Columns for Capillary Electrochromatography Separation

Fritless packed silica gel columns were prepared using sol-gel technology, The part of a 75 μm i.d. capillary was filled with a mixture of methacryloxypropyltrimethoxysilane, toluene and hydrochloric acid. Four different photoinitiators such as benzoin methyl ether, Irgacure 819, Irgacure 1700 and Irgacure 1800 were added in the presence or absence of sodium dodecyl sulfate during the polymerization process. The above eight solutions were irradiated at 365 nm about 5-10 min to prepare the porous monolithic sol-gel columns by a one-step process.

Novel preparation of monolithic imprinted columns for electrochromatographic separation by photopolymerization

A monolithic molecularly imprinted polymer with specific recognition ability for 4-hydroxybenzoic acid (4-HBA) was prepared by in situ photopolymerization, using methacrylic acid (MAA) as a functional monomer, ethylene glycol dimethacrylate (EDMA) as a cross-linking agent, toluene and isooctane as porogenic solvents and Irgacure 1800 as an initiator. Baseline separation of isomers of hydroxybenzoic acid was achieved in less than 8 min on this monolithic column using 4-HBA as template, but not on the blank polymer. Furthermore, some neutral compounds could also be baseline-separated on the imprinted polymer column in the mode of pressure-driven capillary electrochromatography.

Preparation of Polymeric Monolithic Column and Application to the Resolution of Aromatic Compounds in Capillary Electrochromatography

Polymeric monolithic capillary column-poly(GMA-co-EDMA-co-AMPS) was prepared andused for resolution of aromatic compounds (benzalcohol, 2-phenylethanol, toluene, ethylbenzene).

MIL-53-based homochiral metal-organic framework as a stationary phase for open-tubular capillary electrochromatography

Homochiral metal-organic frameworks(MOFs)have attracted considerable attention in many fields of research,such as chiral catalysis and chiral chromatography.However,only few homochiral MOFs can be effectively used in capillary electrochromatography(CEC)and their performances are far from adequate.In this study,we successfully synthesized achiral nanocrystalline MIL-53.A facile post-synthetic modification strategy was then implemented to functionalize the product,yielding a homochiral MOF:L-His-NH-MIL-53.This MOF was then employed as a chiral coating in open-tubular CEC mode(OT-CEC),and,as such,it exhibited high enantioselectivities for several racemic drugs.The homochiral MOF and the fabricated capillary coating were systematically characterized using transmission electron microscopy,scanning electron microscopy(with energy-dispersive X-ray spectrometry),Fourier-transform infrared spectroscopy,X-ray diffractometry,thermogravimetric analysis,circular dichroism spectroscopy,Brunauer-Emmett-Teller surface area measurements,and X-ray photoelectron spectroscopy.This study is expected to provide a new strategy for the design and establishment of MOF-based chiral OT-CEC systems.

A benzenesulfonic acid-modified organic polymer monolithic column with reversed-phase/hydrophilic bifunctional selectivity for capillary electrochromatography

Here,a styrene-based polymer monolithic column poly(VBS-co-TAT-co-AHM)with reversed-phase/hydrophilic interaction liquid chromatography(RPLC/HILIC)bifunctional separation mode was success-fully prepared for capillary electrochromatography by the in situ polymerization of sodium p-styrene sulfonate(VBS)with cross-linkers 3-(acryloyloxy)-2-hydroxypropyl methacrylate(AHM)and 1,3,5-triacryloylhexahydro-1,3,5-triazine(TAT).The preparation conditions of the monolith were optimized.The morphology and formation of the poly(VBS-co-TAT-co-AHM)monolith were confirmed by scanning electron microscopy(SEM)and Fourier transform infrared spectroscopy(FT-IR).The separation perfor-mances of the monolith were evaluated systematically.It should be noted that the incorporation of VBS functional monomer can provideπ-πinteractions,hydrophilic interactions,and ion-exchange in-teractions.Hence,the prepared poly(VBS-co-TAT-co-AHM)monolith can achieve efficient separation of thiourea compounds,benzene series,phenol compounds,aniline compounds and sulfonamides in RPLC or HILIC separation mode.The largest theoretical plate number for N,N0-dimethylthiourea reached 1.7×10^(5)plates/m.In addition,the poly(VBS-co-TAT-co-AHM)monolithic column showed excellent reproducibility and stability.This novel monolithic column has great application value and potential in capillary electrochromatography(CEC).

In situ synthesis of a spherical covalent organic framework as a stationary phase for capillary electrochromatography

Covalent organic frameworks(COFs)are a novel type of crystalline porous organic polymer materials recently developed.It has several advantages in chromatographic separation field,such as high thermal stability,porosity,structural regularity,and large specific surface area.Here,a novel spherical COF 1,3,5-tris(4-aminophenyl)benzene(TAPB)and 2,5-bis(2-propyn-1-yloxy)-1,4-benzenedicarboxaldehyde(BPTA)was developed as an electrochromatographic stationary phase for capillary electrochromatography separation.The COF TAPB-BPTA modified capillary column was fabricated via a facile in situ growth method at room temperature.The characterization results of scanning electron microscopy(SEM),Fourier transform infrared(FT-IR)spectroscopy,and X-ray diffraction(XRD)confirmed that COF TAPB-BPTA were successfully modified onto the capillary inner surface.The electrochromatography separation performance of the COF TAPB-BPTA modified capillary was investigated.The prepared column demonstrated outstanding separation performance toward alkylbenzenes,phenols,and chlorobenzenes compounds.Furthermore,the baseline separations of non-steroidal anti-inflammatory drugs(NSAIDs)and parabens with good efficiency and high resolution were achieved.Also,the prepared column possessed satisfactory precision of the intra-day runs(n=5),inter-day runs(n=3),and parallel columns(n=3),and the relative standard deviations(RSDs)of the retention times of tested alkylbenzenes were all less than 2.58%.Thus,this new COF-based stationary phase shows tremendous application potential in chromatographic separation field.

Recent applications and chiral separation development based on stationary phases in open tubular capillary electrochromatography(2019–2022)

Capillary electrochromatography(CEC)plays a significant role in chiral separation via the double separation principle,partition coefficient difference between the two phases,and electroosmotic flow-driven separation.Given the distinct properties of the inner wall stationary phase(SP),the separation ability of each SP differs from one another.Particularly,it provides large room for promising applications of open tubular capillary electrochromatography(OT-CEC).We divided the OT-CEC SPs developed over the past four years into six types:ionic liquids,nanoparticle materials,microporous materials,biomaterials,non-nanopolymers,and others,to mainly introduce their characteristics in chiral drug separation.There also added a few classic SPs that occurred within ten years as supplements to enrich the features of each SP.Additionally,we discuss their applications in metabolomics,food,cosmetics,environment,and biology as analytes in addition to chiral drugs.OT-CEC plays an increasingly significant role in chiral separation and may promote the development of capillary electrophoresis(CE)combined with other instruments in recent years,such as CE with mass spectrometry(CE/MS)and CE with ultraviolet light detector(CE/UV).

The Synthesis and Characterization of β-cyclodextrin Derivated Pancreatin Used as Chiral Selector in Capillary Electrochromatography

The preparation of capillary electrochromatography column for chiral separation with β-cyclodextrin derivatized Pancreatin was imvestigated, which had three steps, synthesis of β-cyclodextrin derivated pancreatin, the modification of the capillary internal surface and the covalent binding of β-cyclodextrin derivated pancreatin on the capillary internal wall. β-cyclodextrin derivated pancreatin was synthesized using β-cyclodextrin and protein in the presence of ethylene glycol diglycidyl ether （EGDE） in boric acid buffer at pH = 8.7. Amino group was coated on the internal surface of the silica capillary by sot-gel technology using triethoxylmethylsiloxane and （ 3-aminopropyl ） trimethoxysiloxane. Covalent binding of β-cyclodextrin derivated pancreatin was performed by glataraldehyde. Chlorpheniramine, phenylalanine and troopine were separated baseline by β-cyclodetrin derivated pancreatin in capillary electrochromatography.

Determination of N-Methylcarbamate Pesticides in Vegetables by Solid-phase Extraction and Pressurized Capillary Electrochromatography

Capillary electrochromatography （CEC） is a hybrid technique that couples the good selectivity of high-performance liquid chromatography （HPLC） and the high separation efficiency of capillary electrophoresis （CE）. Both charged and uncharged compounds can be separated effectively using CEC. In some cases, however, the bubbles that generated in the capillary column in pure CEC performed on commercial CE instruments will cause unstable current and even disrupt the separation when the concentration of buffer is very high. By applying pressure on the electrochromatographic separation via a micro-HPLC pump, pressurized capillary electrochromatography （ pCEC ） combines two driving factors of the electroosmotic flow （EOF） and the pressure flow, thereby increasing the speed and the selectivity of separation and suppressing the bubble formation. Moreover,

Preparation and Characterization of β-Cyclodextrin Derivatized Ovalbumin Used as Chiral Selector in Pressure Capillary Electrochromatography

Synthesis and properties of β-cyclodextrin derivatized ovalbumin used as chiral selector were investigated, β-cyclodextrin derivatized ovalbumin was synthesized using β-cyclodextrin and ovalbumin in the presence of ethylene glycol diglycidyl ether in boric acid buffer at pH value 8.7 at 37℃. Amino group was coated on the internal surface of the silica capillary by sol-gel technology with triethoxylmethylsiloxane and （3-aminopropyl）trimethoxysiloxane. Covalent binding of g-cyclodextrin derivatized ovalbumin was performed by glutaraldehyde. Enantiomers of chlorpheniramine, phenylalanine and atropine were separated by pressure capillary electrochromatography column coated with β-cyclodextrin derivatized ovalbumin.

Molecularly Imprinted Polymer for Theophylline Retention and Molecular Recognition Properties in Capillary Electrochromatography

Molecular imprinting of theophylline in poly (methacrylic acid- ethylene dimethacrylate) as CEC stationary phases was synthesized by an in situ photo-initiated polymerization reaction. The effect of electrolyte pH on xanthine derivatives and the stability of MIP column performance were investigated. the relative standard deviation (D RS) of migration time of five consecutive runs on MIP column was in the range of 2.2%–3.1%. The reproducibility of migration time column to column of M(A) was in the range of 3.8%–4.9%. The highest column efficiency was more than 140 000 plates per meter. The MIP capillaries had showed better selective for theophylline, which comparing with the reference column. The urine sample was separated by spiked 5×10?4 mol·L?1 theophylline. Key words capillary electrochromatography - molecular imprinting polymers - theophylline CLC number O 657.8 Foundation item: Supported by the National Nature Science Foundation of China (20375028) and the Research Fund for the National High Technology Development “863” of China (2002AA2Z2004)Biography: Cai Ling-shuang (1968-), female, Associate professor, Ph. D, research direction: separation science.

Development of Amine Capillary Column Applied to the Analysis of Basic Compounds by Electrochromatography

An amine capillary column was developed in a fused-silica capillary as stationary phase and applied to separation of basic compounds by capillary electrochromatography (CEC). The functionalized capillary was prepared by inmobilization of 3-Aminopropyl)triethoxysilane (APTES). The CEC conditions including APTES and buffer concentration, pH and applied voltage were investigated to obtain the optimal CEC system for the separation of three anesthetics as basic test molecules. The capillary column provided an efficiency of up to 20,000 plates/m. Lidocaine, ketamine and xilacine were baseline separated under the running conditions with 10 mM Na2HPO4 pH 9.0 as BGE. The applied voltage was 5 kV temperature was set at 25oC and UV detection was performed. The resolutions were 4.97 and 1.53 for ketamine, lidocaine and xilacine, respectively. The column used in CEC mode showed better separation of the anesthetics compared with those used in the capillary zone mode. The comparison with reversed stationary phases used in HPLC in terms of resolution (Rs), sensitivity (LOD), efficiency (N), precision (RSD), asymmetry (T) was also performed. This study provided an alternative way for the CEC separation of basic compounds and demonstrated the improvement in the chromatographic parameters.

Fast preparation of photopolymerized monolithic columns for capillary electrochromatography

Photopolymerized sol-gel(PSG) columns were prepared using methacryloxypropyltrimethoxysilane as the monomer,toluene as the porogen and hydrochloric acid as the catalyst.Four different photoinitiators such as benzoin methyl ether,Irgacure 819,Irgacure 1700 and Irgacure 1800 were comparatively used in the reaction solution in the presence and absence of sodium dodecyl sulfate.The above eight solutions were respectively irradiated at 365 nm for 5?10 min in each capillary(75 μm inside diameter) to prepare the porous monolithic sol-gel column by a one-step,in situ,process.The chromatographic behavior of the eight PSG columns were comparatively studied,all of which exhibit reversed-phase character.Using these columns,several neutral compounds,namely thiourea,benzene,toluene,ethyl benzene,biphenyl and naphthalene can be separated from mixtures with a largest column efficiency of 74 470 plate/column for thiourea.Addition of sodium dodecyl sulfate in the polymerization process has a significant influence on the morphology and migration time.

手性金属有机骨架修饰毛细管硅胶整体柱的制备及其用于手性药物的分离

金属有机骨架材料(MOFs)是一类由金属离子(或金属簇)和有机配体组成的晶体结构化合物。手性MOFs作为一种新型的色谱手性分离材料,已被成功用于拆分手性对映体,表现出良好的手性拆分性能。该研究制备了一种可用于加压毛细管电色谱的手性金属有机骨架修饰毛细管硅胶整体柱。首先,合成了手性金属有机骨架(钴-甘氨酰-L-谷氨酸,Co-L-GG),接着将Co-L-GG作为手性功能单体通过一步原位聚合法制备手性毛细管整体柱。制备手性毛细管整体柱的最佳条件:Co-L-GG用量为5 mg,聚乙二醇用量为0.96 mg,四甲氧基硅烷用量为3.6 mL,甲基三甲氧基硅烷用量为0.4 mL。其次,研究了分离条件对手性药物拆分的影响。在外加电压为-20 kV、流动相为乙腈-20 mmol/L磷酸氢二钠(80∶20,v/v)的条件下,3 min内拆分了6种手性药物,其中氨氯地平、氟伐他汀和色氨酸达到了基线分离。所制备的手性毛细管整体柱表现出良好的重复性和稳定性。最后,使用AutoDock进行分子对接,并借助Discovery Studio对分子对接结果进行分析。结果显示,Co-L-GG与手性药物对映体间的结合自由能差越大,对映体选择性因子越大,然而,这并不一定导致分离度的增加。Co-L-GG中富含伯胺、仲胺和羰基,使其具有对映体识别能力。该研究表明,手性金属有机骨架可用作手性功能单体制备手性毛细管整体柱,在手性化合物的分离和分析中具有广阔的应用前景。

整体柱的制备方法及其应用

整体柱具有渗透性好、制备简单、无需塞子制作等优点 ,从而避免了由塞子所引起的问题 ,已引起人们越来越多的关注。本文对整体柱的制备方法。

毛细管电色谱和加压毛细管电色谱的进展与应用

毛细管电色谱(CEC)以内含色谱固定相的毛细管为分离柱,以电渗流为驱动力,既可以分离带电物质也可以分离中性物质。它结合了毛细管电泳和高效液相色谱两者的优点,兼具高柱效、高分辨率、高选择性和高峰容量的特点,同时具有色谱和电泳的双重分离机理。然而,"纯粹"的电色谱在实际应用中有着天然的弱点,即:在电流通过毛细管柱中的流动相时容易产生气泡(焦耳热作用),从而使电流中断和电渗流停止,毛细管柱必须被重新用流动相润湿后方能再次使用。加压毛细管电色谱(pCEC)将液相色谱中的压力流引入CEC系统中,不仅解决了气泡、干柱等问题,而且实现了定量阀进样和二元梯度洗脱。CEC和pCEC作为微分离领域的两种前沿技术,满足了当前复杂样品分析和分析仪器微型化的需求,近年来获得了广泛的关注。本文综述了这两种技术近来的发展,包括仪器、色谱固定相的发展,总结了其在生命科学、药物分析、食品安全以及环保样品分析等方面的应用进展,评述了各方法的特点,并展望了CEC和pCEC今后的发展和应用前景。

微全分析系统中的电色谱分离技术

微全分析系统(μTAS)近年来发展非常迅速,出现了各种各样思路新颖,设计独特的芯片分析系统。本文着重从分离模式方面介绍了μTAS的一个新的发展方向——电色谱。由于电色谱技术兼具高效液相色谱的高选择性和毛细管电泳的高效性,因此具有广阔的应用前景。