基于液滴微流控接口的高效液相色谱-毛细管电泳二维分离平台初探

蛋白质组体系的高度复杂性需要更高分辨率的多维分离技术。近年兴起的液滴技术在微纳尺度样品操控方面具有微体积、低扩散、无返混等独特优势,有望为多维分离平台的接口提供解决方案。通过采用不同结构的液滴微流控芯片可以实现“液滴生成”与“油相排除”功能,进行样品由连续流-非连续流-连续流的高效转移,将不同的分离模式进行二维耦联。本研究利用液滴作为接口技术耦联高效液相色谱与毛细管电泳构建二维分离系统,以蛋白质降解的复杂多肽混合物为样品,考察了液滴接口二维分离平台的可行性和有效性,并获得3000以上的峰容量,初步展示了该接口技术在多维分离分析领域的应用潜力。     

9-蒽醛衍生化-高效液相色谱法拆分α-氨基酸甲酯和几种脂肪胺对映体

采用高效液相色谱法,以9-蒽醛为衍生试剂,在5种多糖衍生物的手性固定相(CSPs)上对几种α-氨基酸甲酯对映体进行了手性分离。色谱条件如下: 流动相为含3%～10%(v/v)异丙醇的正己烷溶液,流速为1.0 mL/min,检测波长为254 nm。结果表明,α-氨基酸甲酯-9-蒽醛亚胺衍生物在Chiralcel OD柱或Chiralcel OD-H柱上的手性分离结果优于其他CSPs,而且在Chiralcel OD柱或Chiralcel OD-H柱上全部得到了基线拆分(α=1.24～5.47, Rs=2.56～13.90), L-对映体在这两种色谱柱上的保留强于D-对映体。同时还考察了几种脂肪胺在5种多糖衍生物手性固定相上的对映体拆分效果,结果表明脂肪胺的9-蒽醛亚胺衍生物在Chiralcel OD柱或Chiralcel OD-H柱上的分离效果良好。该法可用于其他α-氨基酸酯和胺类化合物对映体的分析。     

正相液相色谱-串联质谱法分离普萘洛尔对映体

建立正相液相色谱-串联质谱(LC-MS/MS)分离普萘洛尔对映体的方法,并用于盐酸普萘洛尔片对映体含量测定.样品使用甲醇进行简单提取,采用Chiralcel OD-H手性柱,以正己烷-乙醇-氨水(70∶30∶0.4, v/v/v)为流动相,流速为0.4 mL/min.在正离子模式下,通过电喷雾离子化(ESI+),采用多...     

单晶菱形CeOHCO3片状物的制备及其向CeO2的热转换

以硝酸铈铵和尿素为反应物,γ-氨丙基三乙氧基硅烷(KH550)为助剂,通过沉淀反应制得了单晶菱形CeOHCO3片状物。然后将CeOHCO3在600℃空气气氛中灼烧获得了菱形CeO2。通过XRD和SEM对反应物中是否含有KH550助剂所得的产物进行了分析,结果发现只有含有KH550才能获得菱形CeOHCO3片状物,并且在灼烧过程中产物的形貌仍保持菱形。然后采用TEM对菱形CeOHCO3和CeO2进行了表征,结果发现CeOHCO3为单晶产物而灼烧后所得的CeO2为多晶产物。     

Liquid Phase Hydrogenolysis of Biomass‐derived Lactate to 1,2‐Propanediol over Silica Supported Cobalt Nanocatalyst

Liquid phase hydrogenolysis of ethyl lactate to 1,2‐propanediol was performed over silica supporting cobalt catalysts prepared by two different methods: precipitation‐gel (PG) technique and deposition‐precipitation (DP) procedure. The cobalt species (Co₃O₄/cobalt phyllosilicate) present in the corresponding calcined PG and DP catalysts were different as a consequence of the preparation methods, and Co OH Co olation and Si O Co oxolation molecular mechanisms were employed to elucidate the chemical phenomena during the different preparation procedures. In addition, the texture (BET), reduction behavior (TPR and in‐situ XRD), surface dispersion and state of cobalt species (XPS), and catalytic performance differ greatly between the samples. Because of small particle size, high dispersion of cobalt species and facile reducibility, the Co/SiO₂ catalyst prepared by precipitation‐gel method presented a much higher activity than the catalyst prepared by deposition‐precipitation method. Metallic cobalt is assumed to be the catalytically active site for the hydrogenolysis reaction according to the catalytic results of both cobalt samples reduced at different temperatures and the structure changes after reaction.     

原子转移自由基聚合法用于以单分散树脂为基质的强阳离子交换色谱固定相的制备及其色谱性能研究

以7μm单分散交联聚甲基丙烯酸环氧丙酯树脂表面键合溴异丁酰溴为引发剂,以CuCl/CuCl2/2,2-联二吡啶(Bpy)为催化体系,采用封闭体系,在氮气保护下,以乙烯基苯磺酸钠(NaSS)为单体、N,N-二甲基甲酰胺(DMF)水溶液为溶剂,制备了强阳离子交换色谱(SCX)固定相,并用元素分析与红外光谱法对其进行了表征....     

苯磺酸氨氯地平对映体在Chiralcel OJ柱上的色谱保留及拆分特性

在Chiralcel OJ手性柱上对苯磺酸氨氯地平对映体进行分离研究.考察了在正己烷流动相体系中,不同碳数、不同立体结构的醇类添加剂以及不同醇含量对分离结果的影响,同时还考察了流速及柱温对分离的影响.并通过色谱保留及热力学行为研究对药物手性识别机理进行了探讨.结果表明,在正己烷-异丙醇(90:10,体积比)为流动相,流...     

左氧氟沙星印迹聚合物微球及其特异吸附研究

以甲基丙烯酸为功能单体,乙二醇二甲基丙烯酸酯为交联剂,采用沉淀聚合法制备了左氧氟沙星印迹聚合物(MIP)微球,用SEM和IR分别对微球形貌和结构进行表征,用静态吸附法和Scatchard分析考察了聚合物微球对模板及其结构类似物的吸附行为和选择性识别能力.结果表明,MIP对模板分子的吸附平衡速度快,40min即可达到吸附...     

Structure and wettability relationship of coelectrospun poly (L‐lactic acid)/gelatin composite fibrous mats

Coelectrospun polylactide(PLA)/gelatin (GE) composite fibrous matrixes have been identified to exhibit much improved performances compared to the respective components; however, the reasons for their water contact angles decreasing to zero at proper PLA/GE ratios remain unclear. To get a deep understanding of the phenomenon, PLA and GE were coelectrospun with different PLA/GE ratios in this study. Although the resulting composite fibers were homogeneous in appearance, they were detected different microscopic structures by transmission electron mircroscope (TEM) and via morphological observations after selective removal of either PLA or GE component. Together with the results of degradation study in phosphate buffered solution, a kind of cocontinuous phase separation microstructure could be identified for the PLA(50 wt%)/GE(50 wt%) composite fibers, which also showed the water contact angle of 0°. This value was far lower than those of electrospun PLA (～123°) and GE (～42°) fibrous matrixes. The X‐ray photoelectron spectrometry (XPS) data revealed that the polar side groups of protein macromolecules have moved toward composite fiber surface with solvent evaporation during electrospinning, due to the hydrophobic interaction between PLA and GE. Then the excellent hydrophilicity of PLA(50 wt%)/GE(50 wt%) composite fibers could be suggested as the consequence of: (1) the cocontinuous phase separation structure could provide more interface and void for water molecules penetrating; and (2) the accumulation of polar groups on composite fiber surface significantly increased the surface wettability. Copyright © 2010 John Wiley & Sons, Ltd.     

Magnetically assisted removal and separation of cationic dyes from aqueous solution by magnetic nanocomposite hydrogels

Magnetic poly(acrylic acid‐acrylamide‐butyl methacrylate) (P(AAB)) nanocomposite hydrogels were prepared and used as adsorbents for removal and separation of cationic dyes from aqueous solution. These magnetic P(AAB) nanocomposite hydrogels were characterized by scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). It was found that these magnetic P(AAB) nanocomposite hydrogels had magnetic responsive characters. The dynamic swelling, removal, and separation of cationic dye, crystal violet (CV), and basic magenta (BM) by these magnetic nanocomposite hydrogels were studied. The adsorption capacity and isotherm studies of cationic dyes onto magnetic P(AAB) nanocomposite hydrogels have been evaluated. The magnetic P(AAB) nanocomposite hydrogels containing Fe₃O₄ particles can be easily manipulated in magnetic field for removal and separation of cationic dyes from aqueous solution. Adsorption process agreed very well with the Langmuir and Freundlich models. Copyright © 2010 John Wiley & Sons, Ltd.