基于木质生物质分级利用的组分优先分离策略

木质生物质是地球上最丰富的一类生物质资源,主要由碳水化合物高分子(纤维素、半纤维素)和芳族聚合物(木质素)组成。木质纤维组分的清洁高效分离,是实现多元化、高值化生物精炼的重要基础。本文首先讨论了基于分级利用的组分分离技术与基于制备纤维素乙醇的预处理技术的不同之处;其次,梳理归纳了五种木质纤维组分优先分级分离策略:纤维素优先分离,木质素优先分离,半纤维素优先分离,木质素和半纤维素优先分离以及纤维素和半纤维素优先分离;再次,基于半纤维素优先分离策略,对国内相关的产业化应用进行了评述;最后,对木质生物质组分分离技术的当下定位和发展前景进行了总结与展望,以期对木质生物质的三大组分有较全面的价值观念和利用思路,并对木质生物质精炼技术的发展提供借鉴与参考。     

离子交换树脂层析法分离木糖醇结晶母液

研究了001系列离子交换树脂抗衡阳离子型式、树脂交联度、树脂粒径等因素对木糖醇结晶母液分离为糖组分和糖醇组分的影响.筛选出了具有较好分离效果的 001×8(Ca)(0.15mm～0.30mm)树脂.对柱温、柱长径比、进料量、进料浓度、洗脱速度、洗脱液pH等操作因素进行了分离条件优化.在优化条件下,对未糖醇结晶母液进行分离,得到去除糖组分的糖醇组分回收率为92.3%,完成了木糖醇结晶母液的阶段性分离纯化任务.     

可调移动重叠分离图法用于高效液相色谱多台阶梯度分离条件优化的研究

计算机辅助高效液相色谱（HPLC）分离条件优化可以低成本、快速地得到优化的分离条,因而已较为广泛地用于复杂样品的分离分析。基于移动重叠分离图方法,又发展了一种新型的多台阶梯度分离条件的优化方法可调移动重叠分离图法。该方法通过预测不同流动相条件下各组分的保留时间、峰宽和分离度,绘制出对于样品中各组分的重叠分离区域图。在对当前台阶流动相组成进行优化的同时,考虑其对后面一到两个台阶上流出组分保留的影响,实时地重新绘制对于后面台阶上流出组分的重叠分离区域图。通过观察当前台阶流动相条件对当前台阶和后面台阶上流出组分分离的影响,综合考虑样品中所有组分的分离情况,找到更接近全局最优的分离条件。通过扫描的方法对优化得到的分离条件进行微调,能够进一步提高分离效果。采用文献数据对可调移动重叠分离图法的应用加以说明,在二元流动相体系下,证明了该方法在HPLC方法建立方面的优越性。     

人血清中核酸组分的反相高效液相色谱分析

核苷酸、核苷和碱基是核酸的主要组分,它们与核酸的代谢有着密切的关系。分离和测定核酸组分的变化在生化和医学上具有重要意义。核苷酸等的分离过去较多地采用阴离子交换法,近年来有用两性离子对HPLC法和反相HPLC法等。本文利用Mg~(2+)对一些组分的配位作用改进了14种最基本核酸组分的峰形和分离度。对人血清中一些核酸组分进行了定性和定量分析。     

催化裂化汽油中含硫化合物的分离氧化脱硫研究

以负载氧化铜的氧化铝层析柱对催化裂化(FCC)汽油全馏分进行分离,使其中的烷烃、烯烃与芳烃、含硫化合物分离成极性不同的两组,含硫化合物在芳烃组分中得以分离富集。分离后对芳烃组分中的含硫化合物进行氧化,脱硫率达72%。氧化后的芳烃组分与分离出来的烷烃、烯烃组分混兑,可使FCC汽油的总脱硫率达71·3%。     

芸芝多糖组分的相对分子质量的凝胶渗透色谱表征

以NaNO3 为主体流动相在Ultrahydrogel水溶性凝胶柱上分离、测定了芸芝多糖组分的相对分子质量。文中讨论了流动相离子强度对吸附的影响 ,从而建立最佳分离、测试条件 ,将芸芝多糖的混合物分离为3个具有生理活性的组分 ,测得各组分的相对分子质量分别为1.19×106;7.96×105;5.52×105。     

一步法和两步法毛细管等电聚焦测定蛋白质和多肽等电点的比较

利用一步法和两步法毛细管等电聚焦(cIEF)方法分离测定了蛋白质和多肽的等电点(pI)。讨论了两步法等电聚焦过程所需的溶液组成、样品进样体积、聚焦电压、聚焦时间和分离条件等因素对分离效果的影响。并对一步法和两步法进行了比较。对细胞色素C、血红蛋白、肌红蛋白、转铁蛋白和牛血清白蛋白以及6种多肽的分析结果表明:一步法步骤简单,分离速度快,可测定单一组分的pI,也能快速分离混合蛋白和多肽,但分离度较差,且不能同时准确测定各组分的pI;两步法步骤复杂,分析时间较长,但能够同时分离并准确测定混合样品中各组分的pI,所测的pI值与单一组分进行测定的结果基本一致。两种方法可相互结合、互为补充,可广泛应用于两性生物微粒等电点的快速和准确测定。     

钢都酒的香味成分分析

通过对钢都酒进行化学处理,分类收集组分,采用GC-MS联用技术对各组分进行分离与定性定量测定,分离并鉴定出35个化合物,并确定了酒的香型。     

酱香型珍酒香气成分的GC/MS分析

对酱香型珍酒进行了化学处理,分类收集组分,将各组分用GC—MS联用法进行分离与定性定量测定。分离出200多个色谱峰,鉴定出了4个化合物。并平行地进行了与茅台酒的对比分析。结果表明此两种酒的主要组分一致,含量接近。     

梯度洗脱优化-离子色谱-脉冲安培法分析婴幼儿配方乳粉中的糖和糖醇

建立了梯度洗脱优化-离子色谱-脉冲安培检测技术分析婴幼儿配方乳粉中麦芽糖醇、半乳糖、葡萄糖、蔗糖、果糖、乳糖6种与代谢疾病紧密相关的糖和糖醇的方法。该方法对样品的前处理、色谱柱的选择、淋洗液的梯度等色谱条件进行了优化,重点研究了淋洗液梯度对各组分分离效果的影响。将梯度洗脱程序分解为弱保留组分分离、乳糖分离、基质消除、系统平衡4个子程序,并分别对其进行了条件优化,实现了6种组分的完全分离,并有效解决了弱保留组分色谱峰易重叠、乳糖色谱峰易拖尾等现象。6种组分的线性范围为0.5~100 mg/L,相关系数（r）>0.99,方法的检出限（S/N=3）为0.06~0.40 mg/L。该方法具有分离度好、灵敏度高等优点,可满足例行分析的要求,同时也为淋洗液的梯度优化提供了可借鉴的方法。     

Resolution of overlapped peaks in liquid chromatography by use of derivative spectrophotometry and multivariate analysis and its application in the determination of active components in insecticide formulations

Two procedures for the determination of active components in insecticide formulations have been devised. The first is based in the use of derivative spectra of the components obtained by a diode-array spectrophotomer around the maxima signal of the chromatographic peak. In the second method, mixtures are resolved by the partial least-squares (PLS) regression method from standard spectra of the pure components; spectra of the components were also registered around the maxima signal of the peak. Both procedures have been applied to the analysis of diverse mixtures of active components (piperonyl butoxide, neopynamine and fenitrothion) in insecticide formulations with satisfactory results.     

电场辐照前后某些中药有效成分的质谱分析

利用快原子轰击质谱（ＦＡＢＭＳ）及解吸电子轰击质谱（ＤＥＩＭＳ）方法，分析了电场辐照前后的５种中药有效成分，证明电场辐照灭菌并不改变其化学结构，讨论了底物效应及正，负快原子轰击质谱的差异，以及与电吸电子轰击质谱的不同断裂规律，同时利用Ｂ／Ｅ联动扫描（亚稳离子测定）进行了验证。     

Thermodynamic behavior of water-acetonitrile mixtures excess volumes and viscosities

Densities of water+acetonitrile mixture have been measured from 308.15 to 278.15 K over the entire composition range. Partial molal volumes of both components of the mixed system have been calculated and deviations from ideal volumes of mixing have been evaluated. Literature data on viscosity have also been treated by a least square method and activation thermodynamic functions of viscous flow computed. Structural correlations have been made with previous results on acid-base properties; they allow to distinguish several interaction regions between components of binary systems.     

A study of the phospholipids of kenaf

Summary The fatty-acid composition of the combined phospholipids and also of the main and two minor components of the phospholipids have been studied. On the basis of the results of acid hydrolysis and also IR spectroscopy, the glycerophospholipid structure of the main components of the total material has been confirmed. These main components have been subjected to enzymatic hydrolysis: the position distribution of the fatty acids have been determined and, from these, the possible diglyceride compositions of the phosphatidylcholines, phosphatidylethanolamines, and phosphatidylinositols have been calculated. It has been shown that the phospholipids are accompanied by 35–40% of carbohydrates which have been characterized qualitatively as disaccharides.Institute of the Chemistry of Plant Substances, Academy of Sciences of the Uzbek SSR, Tashkent. Translated from Khimiya Prirodnykh Soedinenii, No. 3, pp. 289–293, May–June, 1976.     

Electrophoretic investigation of the seed proteins of the cotton plantGossypium hirsutum

The proteins of the buffer-soluble fraction of the seeds of cotton plants of the speciesGossypium hirsutum, wild and ruderal varieties, have been investigated by electrophoresis in polyacrylamide gel and have been subdivided into two classes. Characteristic components have been detected in the protein spectra of these samples. In diploid species of the cotton plant, in addition to characteristic protein components, individual components are also observed.Translated from Khimiya Prirodnykh Soedinenii, No. 5, pp. 736–738, September–October, 1995. Original article submitted November 21, 1994.     

谱图检索结合二级质谱定性分析烟草中挥发性成分

采用同时蒸馏萃取法提取烟叶中的挥发性成分,利用气相色谱-质谱联用仪(GC-MS)分离测定,通过谱库检索和匹配度定性结合色谱保留指数方法鉴定烟叶中挥发性成分,并引入离子阱二级质谱对谱库检索匹配度差距小、含量低,背景干扰大的物质准确定性.采用谱图检索结合二级质谱定性共鉴定144个化合物,其中104个化合物在烟草挥发性成分的文献中已有报道,报道中有9个化合物是通过二级质谱定性,其余40个化合物还未见报道.结果表明,离子阱二级质谱定性的引入提高了对未知化合物定性的准确性和可靠性,适合于烟叶这类复杂植物体系的化学组分研究.     

山苍子核仁油的大口径毛细管柱气相色谱-傅里叶变换红外光谱分析

本文采用国产色谱仪与进口红外光谱仪及接口加工组成气相色谱-傅里叶变换红外光谱(GC-FTIR)分析仪,使用大口径弹性石英毛细管柱(WBC),分析了湖南省永顺县产山苍子核仁油的组成。讨论了利用等高线图(CTD)分析技术及差谱技术处理GC-FTIR分析数据的方法,得出了其中约80多个组分的纯化合物气相红外光谱图,定性了其中38种物质,占总色谱峰面积的90％以上。     

Direct secondary-ion mass spectrometric analysis of mixtures separated by thin-layer chromatography and electrophoresis

Secondary-ion mass spectrometry (SIMS) is used to sputter ions directly from thin-layr chromatograms in which components in a mixture have been separated. Mixtures of phenothiazine drugs and small peptides have been separated an detected by the chromatography/SIMS method. Phosphonium salts have been separated by thin-layer chromatography and imaged in situ by mass spectrometer. Organometallic compounds such as the transition metral acetylacetonates have been simialry determined. Mixtures that have been separated by gel electrophoresis are transferred by using a standard blotting procedure to a nitrocellulose support, which is then examined by secondary-ion mass spectrometry. A mixture of organic dyes was separated by gel electrophoresis, and characterized by secondary-ion mass spectrometry. The use of the mass spectral information to deconvolute overlapping components on the chromatogram is discussed, and the ultimate spatial resolution for molecular mapping is estimated as about 1 μm.     

Isolation methods for the volatile components of grapefruit juice. Distillation and solvent extraction methods

Summary Five different methods including solvent extraction, distillation and simultaneous distillation-solvent extraction (SDE) have been compared for the isolation of the volatile components of grapefruit juice. The search for an adequare procedure was directed to obtaining aroma concentrates with an odour resembling that of the original grapefruit juice. The methods have also been compared in terms of some experimental parameters. The concentrates have been analyzed by fused-silica, capillary gas chromatography and the GC patterns have been compared in terms of the recovery efficiencies for high-, medium-, and low-volatility components. The SDE methods gave the best results, particularly when using the apparatus proposed by Godefrootet al.     

Separation and identification of synthetic dysstuffs by thin-layer electrophoresis and its application in the forensic analysis of liquors

Summary The excessive demand for alcoholic drinks has resulted in the preparation of fakes and created a problem for their identification. Dyestuffs have been added to alcoholic liquors and the separation of these dyestuff mixtures into their various components has been the subject of study by thin-layer electrophoretic techniques on silica gel-G plantes. 10 dyestuffs commonly used in liquors and beverages have been resolved into their components. The migration distances of the separated coloured zones in five electrolytes, either basic or acidic, have been recorded. The technique was found to be particularly suitable for distinguishing fake samples from genuine ones.