Chromatographic separation and recovery of Zn(Ⅱ)and Cu(Ⅱ)from high-chlorine raffinate of germanium chlorination distillation

An anion-exchange-based chromatographic separation approach was developed to selectively recover zinc and copper from the high-chlorine raffinate generated in the process of germanium chlorination distillation using 717 resins based on the coordination difference between Zn^(2+)/Cu^(2+)and Cl^(-).The theoretical calculation and spectroscopic analyses suggested that the coordination between Zn^(2+)and Cl^(-)is much stronger than that between Cu^(2+)and Cl^(-),and the Cl-concentration significantly affects Zn(Ⅱ)and Cu(Ⅱ)species.The factors involving Cl-concentration,resin dosage,shaking speed,and temperature were investigated to determine the optimal condition,and the maximum separation factor of Zn/Cu reached as high as 479.2.The results of the adsorption isotherms,adsorption kinetics,SEM,FTIR,and XPS analyses indicated that the process followed the monolayer uniform chemisorption.Through the continuous adsorption experiments,Zn(Ⅱ)and Cu(Ⅱ)in the high-chlorine raffinate were separately recovered,allowing the reuse of residual waste acid and germanium.

CHROMATOGRAPHIC SEPARATION ON GRAPHITE OF FULLERENE-C_(60) AND-C_(70)

The mixture of fullerene—C_(60) and —C_(70) was successfully separated in larger amount by liquid chromatogra- phy on graphite column.The column was first eluted with a mixture of hexane and toluene,and then with toluene.The eluates were monitored by UV/visible absorption spectroscopy.Graphite column shows high perfor- mance for separation.and much larger quantities of pure C_(60) can be easily obtained. The synthesis of fullerenes(C_(60) and C_(70))in macroscopic quantities has stimulated scientists to study on the method for separating C_(60) and C_(70).Because of the poor solubility of fullerenes C_(60)/C_(70) in most organic solvents,the separation of C_(60) and C_(70) proved to be a challenging task.Most attempts at the separation have used silica and alu- mina as the stationary phase and a mixture of hexane and benzene(or toluene)as the mobile phase. Fullerenes,however,have only limited solubility in hexane,these separations are usually only achieved by limit- ing the amount of sample to a few milligrams.The hexane-silica technique using phenylglycine based HPLC columns appears to offer good separation,but only for submilligram amounts. The use of graphite powder as the stationary phase in liquid chromatography is an advanced separation tech- nique for fullerenes C_(60)/C_(70).The technique is based on that the fullerene-C_(60) is different from C_(70) in the de- gree of electron delocalisation,and C_(60) is much less diamagnetic than C_(70).It is expected that the dissimilarity will cause the C_(60)/C_(70) molecules to exhibit different interactions with graphite,and can be separated from each other on this basis.

HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC SEPARATION OF FULLERENES

High-performance liquid chromatographic systems for the separation of buckminsterfullerene(C_(60)) and related fullerene C_(70) were investigated with methanol/benzene or methanol/toluene (35/65-60/40 in Ⅴ/Ⅴ) as eluant in C18 reversed phase column. The system is suitable for fast analysis of fullerenes at lower percentage of methanol, and repeatly large scale perparation at higher percentage of methanol.

Thin-Layer Chromatographic Separation of Amino Acid Enantiomers using Ligand Exchange

Silica gel thin-layer plates covered with L-arginine and copper acetate were used for the separation of amino acid enantiomers, The chromatographic selectivity and the effects of plate different preparation methods, sample molecular structure and solvent compositions on resolution performance were also discussed.

CHROMATOGRAPHIC SEPARATION OF THE ENANTIOMERS OF 3-PHENYL-1,2-EPOXYETHANE AND 1-PHENYL-1-PROPANOL ON A FUSED SILICA CAPILLARY COLUMN COATED WITH PERBENZYL-β-CYCLODEXTRIN

A β-cyclodextrin derivative, perbenzyl-β-cyclodextrin, was prepared and used as a chiral stationary phase for capillary gas chromatography. Using FID detector and the column temperature between 70 and 80℃, the chiral separations of racemic 3-phenyl-1, 2-epoxyethane and 1-phenyl-1-propanol on a 14m×0.23mm I. D. fused silica column with the β-cyclodextrin derivative were carried out and the optical purities of optically active 1-phenyl-1-propanol samples prepared by asymmetric synthesis were determined.

DETERMINATION OF THERMODYNAMIC AND KINETIC PARAMETERS OF LARGE SCALE CHROMATOGRAPHIC SEPARATION OF SUGAR AND REDUCING SUGAR

The parameter identification model of largr scale chromatography separation process is proposed. The Phase equilibrium constants and lumped mass transfer coefficients of sugar and reducing sugar adsorption on D1, D2 and D3 resins as well as the axial dispersion coefficients of the fluid through packed columns are determined by means of the pulse-response experiment technique with an inert substance as a tracer and the chromatography measuring technique. The elution curve calculated from these parameters is good agreement with the experimental elution curve. The sensitivity analysis of these parameters is carried out, and the ressult shows that the elation curves of chromatography separation are more sensitive to the variations Of the Phase equilibrium relationship than to the variation of the axial dispersion as well as the lumped mass transfer coefficients.

STUDIES ON COUNTERACTING CHROMATOGRAPHIC ELECTROPHORESIS AND ITS UTILIZATION FOR PROTEIN PURIFICATION

A counteracting chromatographic electrophoresis(CACE)separation device has been success-fully built and tested.Experiments are performed with protein mixtures of BSA,Hg,Mg and Cyto-cto study the separation performances,concentration profiles,start-up methodology as well as influ-ences of pH and ionic strength on the separation process.Mathematical models based on the fluiddynamics of the porous medium are proposed.Experiments indicate that the CACE process has agood commercial potential in protein engineering and fine chemicals purification.

Separation and Identification of Glutamine Peptides from Defatted Soybean Meal by Enzymatic Hydrolysis

Glutamine peptides were obtained from defatted soybean meal by enzymatic hydrolysis using a combination of Protamex~? and trypsinase. The results showed that the extent of hydrolysis and the concentration of Gln peptides in the hydrolysate were 22.02%and 6.05 mmol/L, respectively. The hydrolysates were fractionated by size-exclusion chromatography on a Sephadex G-15 into five major fractions(GelF1–GelF5). The peptide(GelF1) fraction with the highest glutamine peptide content(51.8%) was further evaluated to determine its molecular weight distribution. Most(92.37%) peptides were less than 1 000 Da. Glutamic acid and glutamine were the most abundant amino acids, accounting for up to 12.98% of the total amino acid content. In addition, the total amino acid content in GelF1 was higher than that in GelF2 and GelF3.

纳米晶纤维素组装的手性介孔材料及其对手性药物的分离

纤维素纳米晶体(CNC)是由硫酸催化的纤维素水解制备的,根据纤维素的来源和水解条件,纳米晶体的直径约为5~15 nm,长度约为100~300 nm。CNC在水中可以形成具有手性向列型结构的液晶相。当干燥成固体薄膜时,CNC保持螺旋手性向列顺序并组装成层状结构。在CNC自组装过程中,可以添加溶胶-凝胶前体,如Si(OMe)_(4)。随着溶剂的蒸发,这些前体会发生水解和缩合,从而形成手性向列相二氧化硅/CNC复合材料。复合材料在空气中煅烧破坏纤维素模板,留下高表面积手性向列结构的介孔二氧化硅膜。此外,有机二氧化硅或二氧化钛薄膜也采用类似的方法得到。这些薄膜可用作滤光片、反射器和薄膜。最重要的是,合成的手性介孔二氧化硅可用作手性色谱固定相材料分离手性药物。结果显示,手性分离的效果显著,为CNC开发手性新材料提供了新方法。

水蛭素的HPLC色谱分析条件优化研究

为研究水蛭素的HPLC最佳色谱分析条件,通过对比重组水蛭素的HPLC分析方法的洗脱条件、检测波长、色谱柱的分离效果,拟合水蛭素浓度与峰面积的线性方程,优选最佳水蛭素色谱分析条件。结果显示,ODSC18柱分析最佳条件为:采用梯度洗脱,流动相A和B洗脱程序:0~60 min,B:0%~100%,进样量20μL,柱温35℃,流速为1 mL/min,波长205 nm;TSKgelG2000SW柱最佳分析条件为:流动相磷酸缓冲液(0.02 mol/L,pH 7.0),流速0.5 mL/min,检测波长205 nm,进样量20μL。研究表明,水蛭素浓度与峰面积具有良好的直线线性相关关系,采用TSKgelG2000SW色谱柱的分析效果优于ODSC18柱,可为动物活性多肽的分析提供依据。

锂同位素阳离子交换树脂分离纯化方法与应用进展

锂(Li)同位素是良好地球化学示踪工具,被广泛应用于壳幔物质循环、行星起源与演化、大陆风化、古环境与气候变迁、成矿机制及环境污染等领域。然而,分析测试过程中同质异位素的潜在干扰使得自然样品中Li的高效分离纯化成为关键需求。近几十年来,锂同位素阳离子交换树脂分离纯化法得到了广泛应用和发展,形成了多类型不同自然样品中Li分离纯化的一系列方法体系。从早期Li的分离纯化方法仅注重于实现自然样品Li的分离效果,使之满足TIMS分析需求,逐渐发展到注重减少分离纯化过程中引入空白污染、简化操作提高分离效率以及对不同类型自然样品具有广泛适用性等方面。本文阐述了近年来基于阳离子交换树脂法的锂同位素分离纯化方法研究进展,重点总结了单柱法、双柱法、多柱法和套柱法的操作流程与技术特点,从树脂类型选择及用量、淋洗液类型选择及其在不同类型自然样品中的适用性和应用效果等方面,分析了各类方法的应用优势。目前单柱法和双柱法是Li分离纯化研究中应用较为广泛的方法,在不断优化过程中,一些方法的树脂用量低至1mL,淋洗液用量少于10mL,流程空白控制在1‰以下,整个淋洗流程被缩短至数小时之内。但不同分离纯化方法仍在很大程度上依赖于样品Li含量及其他基质离子等因素。因此,在兼顾分离效率、适用范围以及经济性等因素下,进一步优化现有方法体系、扩展不同类型样品适用范围,对于提升锂同位素分析效率和精度以及推动锂同位素应用研究发展具有重要意义。随着测试设备和技术的不断进步,逐步探索自动化淋洗设备在自然样品Li高效分离纯化中的应用,将成为锂同位素分析技术的主要发展方向之一。

用于分离单糖与寡糖的亲水色谱材料制备及应用进展

糖类化合物在食品科学、医药科学、生命科学等领域中发挥至关重要的作用。糖类化合物可分为单糖、寡糖和多糖,其中单糖和寡糖大多是可溶性糖,不仅可以充当结构物质,还具有抗氧化、抗癌、抗菌、抗病毒等多种生物活性。亲水作用色谱弥补了反相液相色谱在糖类化合物分离方面的不足。本文重点介绍了2017—2022年报道的适合分离分析单糖和寡糖的氨基键合固定相、酰胺类键合固定相、糖类键合固定相、两性离子键合固定相等亲水色谱固定相,并概述了乙腈含量、缓冲盐浓度、流动相pH值和柱温等色谱分离条件对亲水分离效果的影响,以期为单糖及寡糖的分离分析提供一定的参考。

顺序式模拟移动床色谱高效纯化低聚异麦芽糖应用研究

[目的]提高低聚糖行业的生产效率。[方法]以50型低聚异麦芽糖浆为原料,利用顺式模拟移动床色谱分离技术对其纯化。通过制备色谱单柱试验筛选出钾离子型树脂为合适的分离介质;根据物料平衡原理和顺序式模拟移动床基本原理近似确定分离工艺的初始操作参数,并对分离条件进行优化。[结果]最佳技术参数为:料液折光率60%、柱温65℃、进样量455 mL、进水量682 mL、进样流量37.4 mL/min、进水流量29.6 mL/min以及总循环流量364 mL/h,在此条件下低聚异麦芽糖出口折光为20.40%,纯度达到90.20%,收率达到85.50%。[结论]自主研制的顺序式模拟移动床色谱分离设备可用于高效纯化低聚异麦芽糖。

色谱技术在抗体分离纯化中的应用进展

抗体作为一类重要的生物药物,在疾病诊断和治疗等方面拥有广阔的前景。抗体药物的需求逐年上升,生产规模不断扩大,下游抗体纯化已经成为抗体药物生产的瓶颈。色谱技术具有选择性好、分离效率高等优点,在抗体纯化领域占据主导地位。抗体分离纯化流程一般包括样品的粗提、粗提物精制和抗体精纯3个步骤,每个步骤都涉及色谱分离技术。目前已有多种色谱技术(如亲和色谱、离子交换色谱、疏水作用色谱、混合模式色谱以及新型的温敏色谱等)应用于抗体的分离纯化。本文介绍了近年来国内外各种色谱技术在抗体分离纯化方面所取得的研究进展,并对抗体色谱分离技术的未来发展趋势进行了展望。

新型多孔材料在黄酮类样品分离检测前处理中的研究进展

黄酮类化合物是一类具有抗炎、抗氧化、神经保护、抗癌、抗菌和抗病毒等多种功效的天然产物,在医药、食品以及化妆品等领域具有广泛的应用。然而,该类物质往往具有相似的结构,且在天然植物中的含量较低,所以其分离和鉴定难度较大。因此,如何获得高纯度的黄酮类化合物产品是该领域研究的热点问题。近年来,金属有机骨架(MOFs)材料和共价有机骨架(COFs)材料所代表的新型多孔材料(POFs)由于具有超高的比表面积以及优异的孔结构特性越来越受到研究者们的重视,在样品前处理及色谱分离中具有巨大的应用潜力。本文综述了MOFs及COFs作为分离材料在样品前处理和分离检测黄酮类化合物方面的研究进展,重点探讨2种POFs材料的结构特点和分离特性,并对其应用前景进行展望,以期为开发新型MOFs和COFs用于天然产物的分离纯化研究提供参考。

亲脂性匹配色谱分离-超高效液相色谱-串联质谱法测定果蔬中21种三唑类杀菌剂

为了提高农药残留的色谱分离效率和降低基质效应,本研究提出亲脂性匹配色谱分离,选取三唑类杀菌剂为研究对象,建立了果蔬中21种三唑类杀菌剂的超高效液相色谱-串联质谱(Ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)检测方法。样品经乙腈提取,盐析分相,分散固相萃取净化,选用与三唑类杀菌剂具有相近亲脂性的色谱柱进行分离,探究不同亲脂性烷基键合相对基质效应、回收率以及三唑杀菌剂和基质组分色谱分离的影响。结果表明,亲脂性匹配色谱分离能够提高色谱分离效率,改善三唑杀菌剂和基质组分的色谱分离,21种三唑杀菌剂的基质效应为-8.3%~4.7%,在5~250μg/L浓度范围内线性关系良好,决定系数R2≥0.999,平均回收率为91.4%~108.1%,定量限为0.5~3.5μg/kg。该检测方法能够有效降低基质效应,使用溶剂校准曲线进行定量即可获得满意的回收率,显著提高了检测效率,具有简便、准确、灵敏度高等特点,适用于果蔬中三唑杀菌剂的检测。所述亲脂性匹配色谱分离,为农药残留的液相色谱-串联质谱法分析中液相色谱柱的选择和基质效应的降低提供了方法参考。

色谱技术在手性药物分离研究中的应用

本文指出目前使用的药物中有一半以上是手性药物,手性药物单一异构体研究已成为新药研发的重点方向;而现代色谱技术具有高分离效率,是手性药物分离领域的常用技术。本文综述了目前手性药物分离的主要色谱技术,包括高效液相色谱法(HPLC)、气相色谱法(GC)、毛细管电色谱法(CEC)、高速逆流色谱法(HSCCC)和超临界流体色谱法(SFC)的原理和应用,为手性药物的分离需求提供参考。

气相色谱法分析草酸二甲酯纯度方法改进研究

DMO国标分析方法采用毛细色谱柱进行分析,在国标方法使用过程中没有提到空白计算方法,使分析结果和实际样品有差别。在分析过程中由于仪器有细微差别,组分分离度不好,DMO出现过载现象,为了使各组分色谱峰出峰的有效分离,排除干扰,对柱流量和分流比及进样方式进行了改动,使各个组分有效分离,消除DMO因进样产生的过载现象。

离子色谱法中色谱分离面临的挑战与对策

离子色谱法作为一种重要的分离分析技术,在环境、食品、生物医药等领域具有广泛应用。然而,色谱分离过程中面临着诸多挑战,如复杂样品矩阵的干扰、色谱柱的选择性与寿命问题、流动相的优化难题等。本文综述了离子色谱法中色谱分离所面临的挑战,并提出了相应的对策,旨在提高色谱分离的效果和效率,推动离子色谱法在更多领域的应用和发展。

双柱箱气相色谱仪在裂解气组成分析中的应用

阐述了裂解气组成分析的重要意义。采用2台气相色谱仪并联的方式,将2个十通阀、3个六通阀、7根色谱分析柱、2个热导池检测器(TCD)和1个氢火焰离子化检测器(FID)合理配置在2台色谱仪主机内部。利用分流进样方式、三通道并行、双检测器检测、阀位切换、程序升温以及色谱柱反吹技术,通过3条系统流路输出检测结果,实现了在20 min之内乙烯装置裂解气组成中一氧化碳、二氧化碳、硫化氢、氢气、氮气、氧气以及C_(1)~C_(6)共计22种组分的一次性快速分离,然后利用外标法进行定量计算。结果表明该方法具有分离效果好、操作简便、分析速度快、定量准确和重复性好的优点。