树脂吸附层析法分离喜树果中的喜果甙

自 1 96 6年 Wall等 [1] 首次从喜树植物中分离出喜树碱后 ,至今已有 2 0多种化学成分从中分离出来 ,包括喜树碱 (Camptothecine,CPT)、 1 0 -羟基喜树碱、 1 1 -羟基喜树碱、 1 0 -甲氧基喜树碱、喜树次碱、白桦脂酸及喜果甙 (Vincoside- lactam,VCS- LT)等 [2 ] .研究表明 ,喜树碱类化合物和喜果甙均具有抗癌活性 [3～ 5] .从喜树果中分离喜果甙对充分利用我国丰富的喜树资源具有重要意义 .目前文献报道的分离提取喜果甙方法主要是溶剂萃取和氧化铝柱层析法 [6] ,过程复杂 ,收率很低 .本文采用树脂吸附法对喜果甙进行分离纯化 ,再经…     

胺化超高交联吸附树脂的制备及其对喜树碱和喜果苷的色谱分离

胺化超高交联吸附树脂的制备及其对喜树碱和喜果苷的色谱分离;喜树碱;喜果苷;胺化超高交联吸附树脂;吸附性能;层析分离     

大孔吸附树脂提取喜树碱的研究

本文研究了大孔吸附树脂提取喜树碱的方法，包括树脂的筛选，喜树碱溶液的浓度、温度、ＰＨ值和盐离子浓度对吸附的影响，解吸剂的选择，解吸剂的ＰＨ值、流速对解吸的影响。确定了适宜的吸附和解吸条件。     

大孔吸附树脂合成及从甜叶菊中提取分离甜菊甙的研究

本文合成了一系列用于从甜叶菊提取液中吸附分离甜菊甙的大孔吸附树脂，测定了它们的孔结构参数及吸附量，并比较了吸附量较高的五种树脂的循环使用性能及解吸性能。实验结果表明，Ｍ－３５树脂吸附量大，解吸率高，用树脂法工艺制备的甜菊甙产品纯度高，质量好。     

含酮基吸附剂对莱鲍迪甙A的吸附选择性研究

合成了一系列具有不同骨架结构的中极性含酮基大孔吸附树脂，研究了树脂极性与骨架结构的关系，讨论了树脂对甜菊糖中两种主要糖甙甜菊甙及莱鲍迪甙Ａ的吸附能力和吸附选择性，并设计通过树脂柱的动态色层法从甜菊甙含量高的甜菊糖中成功地分离出高莱鲍迪甙Ａ糖产品．     

大孔吸附树脂处理含磺胺废水的研究

利用大孔吸附树脂处理含磺胺废水。实验表明，DRHⅢ树脂对磺胺具有良好的吸附－解吸效果。原废水中磺胺浓度约为17.2g/L,COD约为13750mg/L，经树脂吸附处理后，废水中COD去除率约86％，磺胺的吸附率88．2％，树脂的解吸率为97．5％，磺胺的回收率约86．0％，其纯度达99．8％。在废水有效处理的同时实现了废物资源化，具有良好的环境效益和较高的经济效益。     

吸附树脂AB—8对甜菊甙的吸附性能及在其提取纯化中的应用

考察了大孔吸附树脂ＡＢ－８对甜菊甙的吸附性能，和溶液的ＨＰ值，洗脱剂的种类及流速对树脂吸附，脱附性能的影响，结果表明，ＡＢ－８树脂对甜菊甙吸附量高，循环使用性能好且易于洗脱。     

树脂吸附法处理异丙隆生产过程中含异丙隆废水的研究

本文用CHA—101树脂处理异丙隆生产过程中的含异丙隆废水,控制泄漏点在异丙隆浓度为140mg/l时,树脂可处理废水36BV,树脂工作吸附量约70mg/ml,树脂的吸附率达95％,吸附后废水经试验可完全套用到生产异丙隆工段中去,实现了闭路循环。树脂吸附饱和后,用工业酒精能基本脱附异丙隆。     

若干极性树脂对黄芩甙及黄芩黄素的吸附性能研究

测定了35种具有不同极性的吸附树脂对黄芩甙及黄芩黄素的吸附量,发现弱碱树脂具有较大的吸附量,研究了弱碱树脂对黄芩黄素的吸附动力学,观察到该树脂对黄芩黄素的吸附较快,5h已基本达到吸附平衡。     

吸附树脂的色层吸附及其在甜菊甙分离纯化中的应用

研究了ADS－7等吸附树脂对甜菊甙各组分的吸附选择性及色层吸附性能,发现ADS－7吸附树脂不仅在吸附甜菊甙时对各个组分呈现出一定的选择吸附顺序,在水洗时还有一定的选择洗脱顺序,这两个顺序正好相反。利用ADS－7吸对脂的这一色层性能,制备了富含甜度最高、味质最好的Rebaudioside A及几科不含色素的高品质甜菊甙,具有很好的实际应用意义。     

聚丙烯酰胺型配体交换色谱载体的合成及分离氨基酸

合成了以亲水性聚丙烯酰胺为骨架的含有可与铜离子形成五元环螯合物配位基团的螯合树脂,这些树脂的Cu~(2+)络合物作为配体交换色谱载体对中性氨基酸进行了分离,并与2种已知螯合树脂的Cu~(2+)络合物作为载体的色谱行为作了比较。本文合成的树脂具有最好的分高性能,研究了色谱条件对分离的影响,讨论了色谱分离机制。     

Effect of the content of divinylbenzene in ion-exchange resins on the chromatographic separation of alpha-cyclodextrin and glucose

In the chromatographic separation of alpha-cyclodextrin and glucose, the parameters relating to the adsorption equilibria and rate processes of the solutes were evaluated for the sodium forms of cation-exchange resins with contents of divinylbenzene (DVB) of 2, 4, 6 and 8%. By using these parameters, the chromatograms of the solutes were then calculated. It is concluded that the resin with 6% DVB is most suitable for the chromatographic separation of the solutes on a preparative scale.     

聚甲基丙烯酰胺型配体交换色谱载体的研究

通过交联聚甲基丙烯酸甲酯与过量的乙二胺或多乙烯多胺反应,然后再与氯乙酸反应得到含有α-胺基乙酸基团的亲水性的聚甲基丙烯酰胺树脂.用这些树脂的Cu~(2+)络合物作为色谱载体对中性氨基酸进行分离.研究了色谱条件如洗脱剂组成、流速和柱温对分离的影响.     

Preparation of monodispersed vinylpyridine–divinylbenzene porous copolymer resins and their application to high-performance liquid chromatographic separation of aromatic amines

For the separation of aromatic amines, two types of monodispersed porous polymer resins were prepared by the copolymerization of 2-vinylpyridine and 4-vinylpyridine with divinylbenzene in the presence of template silica gel particles (particle size 5 μm), followed by dissolution of the template silica gel in an alkaline solution. The transmission electron micrographs and the scanning electron micrograph revealed that these templated polymer resins have a spherical morphology with a good monodispersity and porous structure. Using these monodispersed polymer resins, the high-performance liquid chromatographic separation of aromatic amines in the mobile phases of pHs 2.0, 2.9, 4.1, 7.2 and 11.7 were carried out. The 2-vinylpyridine–divinylbenzene copolymer resins showed slightly stronger retentions for aromatic amines than the 4-vinylpyridine–divinylbenzene copolymer resins. Under acidic conditions (around pH 2.0), aniline and the toluidines showed no retention on these copolymer resins due to the repulsion between the cationic forms of these amines and pyridinium cations in the stationary phase, whereas less basic aromatic amines or non-basic acetanilide showed slight retentions. Above pH 4.1, the separation of aromatic amines with these polymer resins showed a typical reversed-phase mode separation. Therefore, the separation patterns of aromatic amines are effectively tunable by changing the pH value of the mobile phases. A good separation of eight aromatic amines was achieved at pH 2.9 using the 2-vinylpyridine–divinylbenzene copolymer resins.     

高效液相色谱法测定水性酚醛树脂中残留的甲醛和苯酚

采用高效液相色谱法同时测定了水性酚醛树脂粘稠液体中残留的甲醛和苯酚,用2,4-二硝基苯肼对甲醛进行衍生化,然后进行色谱分离。色谱柱:Waters Symmetry C18 (5 μm,4.6 mm × 250 mm);柱温:30 ℃;流动相:甲醇-水(体积比为43∶57);检测波长:苯酚270 nm,甲醛360 nm;运行时间:45 min;流速:0.8 mL/min。方法的相对标准偏差小于5%,检测限小于1 μg/L,加标回收率为96%~105%。使用该分析方法可对该类树脂的质量性能进行有效监控。     

Preparative purification of salidroside from Rhodiola rosea by two‐step adsorption chromatography on resins

Salidroside is an effective adaptogenic drug extracted from Rhodiola species. In the present study, a simple and efficient method for preparative separation and purification of salidroside from the Chinese medicinal plant Rhodiola rosesa was developed by adsorption chromatography on macroporous resins. The static adsorption isotherms and kinetics of some resins have been determined and compared for preparative separation of salidroside. According to our results, HPD‐200 resin is the most appropriate medium for the separation of salidroside and its adsorption data fit the Langmuir isotherm well. Dynamic adsorption and desorption were carried out in glass columns packed with HPD‐200 to optimize the separation process. After two adsorption and desorption runs, a product with a salidroside content of 92.21% and an overall recovery of 48.82% was achieved. In addition, pure lamellar crystals of salidroside with a purity of 99.00% could be obtained from this product. Its molecular weight was determined by an ESI‐MS method. The simple purification scheme avoids toxic organic solvents used in silica gel and high‐speed counter‐current chromatographic separation processes and thus increases the safety of the process and can be helpful for large‐scale salidroside production from Rhodiola rosea or other plant extracts.     

Development of a relatively cheap and simple automated separation system for a routine separation procedure based on extraction chromatography

A robust analytical method has been developed in our laboratory for the separation of radionuclides by means of extraction chromatography using an automated separation system. The proposed method is both cheap and simple and provides the advantageous, rapid and accurate separation of the element of interest. The automated separation system enables a shorter separation time by maintaining a constant flow rate of solution and by avoiding clogging or bubbling in the chromatographic column. The present separation method was tested with two types of samples (water and urine) using UTEVA-, TRU- and Sr-specific resins for the separation of U, Th, Am, Pu and Sr. The total separation time for one radionuclide ranged from 60 to 100 min with the separation yield ranging from 68 to 98% depending on the elements separated. We used ICP-QMS, multi-low-level counter and alpha spectroscopy to measure the corresponding elements.     

New SPE column packing material: Retention assessment method and its application for the radionuclide chromatographic separation

The preparation of the OASIS?-HLB sorbent based solid phase extraction (SPE) resins and their application for the ¹⁷⁷Lu radioisotope separation were investigated. Di-(2-ethylhexyl) orthophosphoric acid (HDEHP) impregnated OASIS-HLB sorbent based SPE resins (OASIS-HDEHP) were successfully developed from this investigation. The wettable porosity structure of the moderately extractant impregnated OASIS-HDEHP resins is favorable for the effective diffusion of polar and ionic solutes giving good separation performance. Its good wetting ability offers ease of packing into conventional chromatographic columns. Their off-gassing-free operation makes OASIS-HDEHP columns good for long term use with highly consistent elution dynamics (several dozens of separations perfectly achievable on the same column). The simple method for the capacity factor (k’) evaluation was developed to facilitate the characterization of the SPE chromatographic resin column. A competent procedure using OASIS-E30RS resin (one member of the OASIS-HDEHP resin group) for the separation of no-carrier added (n.c.a) ¹⁷⁷Lu from the bulk amount of Yb target was developed. This separation procedure has showed very good performance with several prominent advantages such as the much shorter separation time (5–6 hours) and high reproducibility. Its high adsorption capacity for Yb and Lu makes it ideal for the separation of the bulky sample (50 mg Yb target for the 20 g weight resin column) for the production of the several Ci of ¹⁷⁷Lu radioactivity.     

Co-eluent effect in partition chromatography. Rhamnose-xylose separation with strong and weak cation-exchangers in aqueous ethanol

The effect of ethanol in aqueous eluent on the chromatographic separation was studied at 298 K. Two sugars, L-rhamnose and D-xylose, were separated by using strong and weak cation-exchangers as a stationary phase. The ionic form of the resins was Na+ or Ca2+. The separations were carried out with sugar feed concentrations up to 35 wt% and with both low (about 1%) and high (about 10%) feed volume to bed volume ratios. The separation of the sugars was improved by adding ethanol into the eluent. The separation was also significantly enhanced when the weak cation-exchangers with the greatest affinity for water were used instead of strong cation-exchangers as a separation medium for the sugars having different hydrophilicities. The experimental data were successfully explained with a rate-based column model, which accounted for the volume changes of the stationary phase. A thermodynamic sorption model was utilized in column calculations.     

Pyrolysis-gas chromatography-mass spectrometry of cured phenolic resins

A previously described pyrolysis device with a movable reaction zone was used in the present work for thermal degradation of cured novolac and resol resins. After the pyrolysis the usual major components were identified, as well as relatively low-volatile aromatic compounds which were revealed after their separation in a capillary chromatographic column. Among the latter components, for both types of cured resins, xanthene and its methyl derivatives were found. The isomers of bis(hydroxyphenyl)methane were found in considerable quantities only in the case of partially cured novolac resins which contained any linear sequences in their structure.