台锥形柱尾的填充毛细管液相色谱柱

首次将台锥形柱尾用于填充毛细管液相色谱柱,并与环氧胶粘的柱尾连接方式进行比较,发现在柱内径≥０．３２ｍｍ时,前者的柱效比后者高出３０％～５０％,且明显改善柱效－流速特性。对比研究了不同内径柱（０．５３ｍｍ,０．３２ｍｍ,０．２５ｍｍ）采用两种尾接方式的塔板高度与流速的关系,对产生差异的原因进行了探讨。     

电填充毛细管色谱柱性能的评价

报道了一种毛细管色谱柱的电填充技术,并进行了柱性能的评价研究。实验表明新的填充方法确保了色谱柱的柱效和重现性。     

Study of Removal of Cationic Dye from Waste Aqua Using Chromatographic Grade Silica as Adsorbent

The adsorption of cationic dye, Basic Red 13 from aqueous solution onto silica has been studied. The time growth adsorption as a function of the amount of adsorbent, pH, initial dye concentration as well as the temperature was measured of the system. Adsorption was found to follow a first-order process. Various isotherm and thermodynamic parameters for the adsorption of dye have been calculated. Isotherms were used to identify formation of either monolayer or multilayer formation whereas thermodynamic and other parameter indicated that the dye adsorption process was physisoption as well as spontaneous and exothermic in nature.     

不锈钢宽口径填充毛细管液相色谱柱

 设计了一种零死体积的二通式柱尾结构和一种使匀浆填料均匀进入色谱柱管内的储料池 ,研究了制备内径在 0 5mm～ 1 0mm的不锈钢宽口径填充毛细管液相色谱柱的方法。详述了以不同牌号、规格的反相ODS类固定相制备的不同柱长的色谱柱的性能。通过折合板高 /折合流速关系和不对称因子对柱性能进行了评价 ,结果表明 ,该方法制备的色谱柱柱效达到理论值的 75 %以上、RSD为 6% ,稳定性也很好。将其应用于抗癫痫药物和氯苯类化合物的分析 ,结果令人满意。     

不锈钢宽口径填充毛细管液相色谱柱的制备及评价

设计了一种零死体积的柱尾连接方式和一种能使匀浆填料均匀进入色谱柱管内的锥形储料池。详述了以反相 ＯＤＳ为固定相,制备高效稳定的不锈钢宽口径（０．８ ｍｍＩ．Ｄ．）填充毛细管液相色谱柱的方法。系统地考察了填装方向、加压溶剂、匀浆溶剂、匀浆浓度和填装压力等不同因素对柱效的影响。在４０ＭＰａ压强和优化条件下,可重复制得柱效达理论塔板数为７．５×１０４／ｍ。对所测试的样品,色谱峰不对称因子为１．０３～１．１０。     

高聚物型色谱柱在高效液相色谱法分离测定有机酸中的应用

考察高聚物型色谱柱(聚苯乙烯-二乙烯基苯,PS-DVB)分离5种有机酸标准品以及琥珀酸发酵液中5种成分的适用性。采用MKF-YJS色谱柱(250mm×4.6mm,5μm),流动相为0.02mol·L-1磷酸二氢铵溶液(用磷酸调pH至2.5)与乙腈以体积比97比3组成的混合溶液;流量1.0mL.min-1;柱温25℃;检测波长为210nm。结果表明:5种有机酸标准品以及琥珀酸发酵液中5种成分均达到了良好的分离效果;琥珀酸质量浓度在0.05～12.0g.L-1范围呈线性,琥珀酸的检出限(3S/N)为0.005g.L-1;进样精密度0.63%(n=5);发酵液中琥珀酸平均回收率为91.8%。     

Cationic Lanthanide Luminescent Copolymer: Design,Synthesis and Interaction with DNA

Polymerizable rare earth complex Eu(AA)₃Phen was synthesized by complexion of europium ion, acrylic acid (AA), and 1,10-phenanthroline (Phen). The structure and fluorescence properties of the complex were studied by elemental analysis, ¹H-NMR spectroscopy, and fluorescence spectroscopy. Eu-containing copolymer poly(PEGMA-co-MMA-co-METAC-co-Eu(AA)₃Phen) (PPMMEu) was then synthesized by free radical copolymerization of Eu(AA)₃Phen and other functional monomers including poly(ethylene glycol) methyl ether methacrylate (PEGMA) and [2-(Methacryloyloxy) ethyl] trimethylammonium chloride (METAC). ¹H-NMR spectroscopy and fluorescence spectroscopy were used to characterize the copolymer and the interactions between the copolymer and DNA was investigated by TEM, fluorescence spectroscopy, and agarose gel electrophoresis. The desired luminescent cationic copolymer was successfully obtained. The copolymer can form micelles in water solution and can efficiently bind to DNA molecules through electrostatic interaction. The results suggest the potential use of PPMMEu in bioprobes and gene vectors.     

High Performance Liquid Chromatography Separations Using Short Columns Packed with Spherical and Irregular Shaped ODS Particles

Abstract

In a comparative study of the separation of a mixture of polycyclic aromatic hydrocarbrons on 5 cm and 10 cm columns packed with 3μ and 5μ ODS spherical particles, the separations achieved on the 10 cm column were not significantly better than those on the 5 cm column. Although, columns packed with 3μ ODS spherical particles gave slightly better resolution than those packed with 5μ ODS spherical particles having the same physical properties, differences were observed when columns packed with ODS spherical particles were compared with columns packed with ODS irregular shaped particles of the same size.

The results show that separations on a 5μ or 3μ packed columns takes place at the first few centimeters.     

Ligand Fishing with Cellular Membrane-Coated Magnetic Beads: A New Method for the Screening of Potentially Active Compounds from Natural Products

Ligand fishing with target biomolecule-immobilized magnetic beads (MBs) has been established and developed for nearly 10 years. Advantages of this technique, such as the ease of operation, associated with a diversity of automated online approaches, make it a valuable tool for affinity studies. However, transmembrane proteins have not been used as the target biomolecules in the assay, since they are usually not available in a purified and bioactive form. In addition, few publications have reported the use of this method for screening active compounds derived from natural products. In this work, for the first time, cellular membrane-coated MBs, which to a large extent maintain the activity of the transmembrane proteins, were used for the fishing assay. We demonstrated application of red blood cell membrane-coated MBs for fishing potential active components from a natural product (Angelica dahurica). The potential active compounds, such as imperatorin, bergapten, and pabulenol, were detected. The result correlated well with cell membrane chromatography (CMC) coupled with HPLC. Comparisons of the developed MBs fishing assay with the CMC method showed the noteworthy advantages of the fishing technique regarding the consumption of cellular membranes, buffers as well as length of operation time.     

Heavy Metal Removal from Synthetic Solutions with Magnetic Beads Under Magnetic Field

The aim of this study is to prepare magnetic beads which can be used for the removal of heavy metal ions from synthetic solutions. Magnetic poly(ethylene glycol dimethacrylate‐vinyl imidazole) [m‐poly(EGDMA‐VIM)] beads were produced by suspension polymerization in the presence of magnetite Fe₃O₄ nano‐powder. The specific surface area of the m‐poly(EGDMA‐VIM) beads was found to be 63.1 m²/g with a size range of 150–200 µm in diameter and the swelling ratio was 85%. The average Fe₃O₄ content of the resulting m‐poly(EGDMA‐VIM) beads was 12.4%. The maximum binding capacities of the m‐poly(EGDMA‐VIM) beads were 32.4 mg/g for Cu²⁺, 45.8 mg/g for Zn²⁺, 84.2 mg/g for Cd²⁺and 134.5 mg/g for Pb²⁺. The affinity order on mass basis is Pb²⁺>Cd²⁺>Zn²⁺>Cu²⁺. Equilibrium data agreed well with the Langmuir model. pH significantly affected the binding capacity of the magnetic beads. Binding of heavy metal ions from synthetic wastewater was also studied. The binding capacities were 26.2 mg/g for Cu²⁺, 33.7 mg/g for Zn²⁺, 54.7 mg/g for Cd²⁺ and 108.4 mg/g for Pb²⁺. The magnetic beads could be regenerated up to about 97% by treating with 0.1 M HNO₃. These features make m‐poly(EGDMA‐VIM) beads a potential candidate for support of heavy metal removal under magnetic field.     

Preparation of Monolithic Capillary Chromatographic Columns Using Supercritical Fluid as a Porogen Solvent

Monolithic polymeric beds were synthesized in fused silica capillaries using either trimethylolpropane trimethacrylate (TRIM) or a mixture of butyl methacrylate (BMA) with ethylene glycol dimethacrylate (EDMA) as monomers. Carbon dioxide at temperature and pressure conditions above its critical values was used as a porogen solvent. The purpose of using the supercritical carbon dioxide was to have the possibility of changing the solvation power (and thus the porosity of the resulting monolith) of the porogen by pressure and temperature changes instead of changing the porogen composition. The experiments were performed using a special setup consisting of a stainless steel high-pressure reactor to which the fused silica capillary was connected. The synthesized monoliths underwent liquid chromatographic evaluation. The polyTRIM capillary monoliths were characterized by different permeability, which depended on the pressure of the synthesis. BMA/EDMA columns were applied for separation of alkylbenzenes and a model mixture of proteins.     

Gas Chromatographic Separation of Carbonyl Compounds as Their 2,4-dinitrophenylhydrazones Using Glass Capillary Columns

The gas chromatographic separation of 22 carbonyl compounds as their 2,4-dinitrophenylhydrazones was investigated using glass capillary columns. Complete separation of the 2,4-dinitrophenylhydrazones of ten aliphatic aldehydes, eight aliphatic ketones and four aromatic aldehydes was obtained, except for the derivatives of n-valeraldehyde and isobutyl methyl ketone, whose peaks overlapped, and the o- and m-tolualdehyde derivatives, which were poorly separated. The optimum conditions were as follows: stationary phase, SF-96; column size, 20 m × 0.25 mm I.D. ; column temperature, 200-240°; injection and detector temperatures, 280-290°; carrier gas flow-rate, helium 1.0-1.2 ml/min or nitrogen 1.1-1.2 ml/min. The method was applied to the analysis of aliphatic carbonyl compounds in car exhaust fumes and cigarette smoke.     

Removal of Anionic Dyes from Aqueous Solution with Layered Cationic Aluminum Oxyhydroxide

It is highly desired yet challenged to find an adsorbent with low cost and excellent performance in the removal of organic dyes from aqueous solution. Here we reported that a layered cationic aluminum oxyhydroxide material hydrothermally synthesized from the low-cost source materials of AlCl₃∙6H₂O, CaO and H₂O, known as JU-111, can meet such criterion in removing methyl orange(MO) and Congo red(CR). JU-111 shows fast adsorption kinetics[especially for CR(15 s)] and high adsorption capacity(MO:>1000 mg/g; CR:>2900 mg/g), surpassing most of the reported adsorbents. Comprehensive characterizations of the adsorption process of MO and CR revealed that both adsorptions were achieved via the anion exchange process. The characteristics of extremely low cost and excellent performance render JU-111 great potential in the practical applications in the removal of anionic dyes.     

苯酚和草酸二甲酯酯交换反应产物的气相色谱分析

提出了苯酚和草酸二甲酯酯交换合成碳酸二苯酯反应的终产物碳酸二苯酯和中间产物草酸二苯酯的气相色谱分析方法 ,采用OV 10 1色谱柱基线分离了碳酸二苯酯、草酸二苯酯及其相关化合物 ,外标法定量测定了碳酸二苯酯和草酸二苯酯 ,其相关系数分别为 1.0 0 0 3和 0 .995 0 ;方法的标准偏差RSD分别为 3.42 %和2 .5 8%;回收率分别为 93.3%～ 10 4.0 %和 95 .0 %～ 10 4.0 %;检出限分别为 8.1× 10 - 2 和 7.7× 10 - 2 g L。     

苯酚和碳酸二甲酯反应产物的气相色谱分析

苯酚和碳酸二甲酯反应产物的气相色谱分析;碳酸二苯酯;碳酸二甲酯;气相色谱     

高效细内径毛细管电色谱填充柱的制备

发展了一套毛细管填充柱制备方法,在１００μｍ内径毛细管柱中填充３μｍＯＤＳ固定相,以毛细管电色谱法（ＣＥＣ）分离模式对芳香胺类样品进行分离,柱效高达２５．９万理论塔板数／米,折合塔板高度达１．３。类似研究在国内尚未见报道。     

溶质在动态改性氧化锆液相色谱柱上的保留行为

分别采用硬脂酸、环糊精和十二烷基磺酸钠动态改性自制的ZrO2微球,研究了流动相中甲醇和改性剂浓度对苯酚及苯甲酸的衍生物、苯胺衍生物及芳香烃类化合物的色谱保留行为的影响。中性及碱性化合物的保留时间较短,色谱峰对称;酸性化合物保留时间较长,色谱峰拖尾较严重。改性氧化锆表现出反相色谱性能。     

Removal of Rhodamine-B from Aqueous Solution by Adsorption onto Crosslinked Alginate Beads

The biosorption of rhodamine-B from aqueous solution using crosslinked alginate beads was studied by contact method at fixed pH ?3 and room temperature (28 ± 0.2°C). Both the Freundlich and Langmuir isotherm models could describe the adsorption equilibrium of the rhodamine-B onto crosslinked alginate beads. The influence of various experimental parameters such as pH, temperature, effect of concentration and time were evaluated. It was observed that the adsorption capacity of rhodamine-B onto alginate beads decreased with increase in pH and temperature above room temperature.     

聚合物基质高效液相色谱填料在白细胞介素-2分离中的应用

聚合物型苯乙烯-二乙烯基苯(PS-DVB)微球装填的麦科菲反相高效液相色谱柱(MKF-RP-HPLC),用于白细胞介素-2(IL-2)分离的最佳色谱条件:流动相A:0.1%三氟乙酸,流动相B:80%乙腈 0.1%三氟乙酸.B液在30 min内从0%线性增大至100%,流速1.0 mL/min;检测波长:280 nm.在该色谱条件下进行系统性实验,结果表明:MKF-RP色谱柱分离IL-2的柱效、分离度、重复性和拖尾因子均能达到药典要求,且柱效和分离度与SOURCE色谱柱相当;MKF-RP色谱柱的pH适用范围为1～14;柱压与SOURCE色谱柱相当,且低于Hypersil C8色谱柱和Polaris C18色谱柱的柱压,可在更高流速下操作;MKF-RP色谱柱的非极性与SOURCE色谱柱相当;MKF-RP色谱柱的超载性能优于SOURCE色谱柱,其对IL-2进样液的最大载样量为300 μg.     

毛细管电泳-激光诱导荧光法分离检测DNA片段及基因扩增产物

以羟丙甲基纤维素和非交联聚丙烯酰胺浴液为筛分介质,将毛细管电泳-激光诱导荧光法用于DNA片段及基因扩增产物的分离检测。探讨了非胶筛分介质中高分子化合物的浓度、电解质的浓度、内插试剂用量等对DNA片段分离检测的影响;考察了DNA片段迁移时间和峰面积的重现性及DNA片段定量检测的关系。建立了一种快速、灵敏的DNA片段及基因扩增产物分离检测方法。