单一阴离子交换柱同时分离有机酸和无机阴阳离子

研究了用乙二胺四乙酸（ＥＤＴＡ）作淋洗液时，性质迥异的有机酸、无机阴离子和碱土金属离子（Ｃａ＾２＋、Ｍｇ＾２＋）在同一阴离子交换柱上的同时分离以及保留机理，结果表明，在离子交换机理之外，非离子交换机理对有机酸及钙镁的ＥＤＴＡ络阴郭的保留行为起一定的辅助作用，９种有机酸和无机阴阳离子在１０ｍｉｎ内得到了较好的分离。各离子的电导检测灵敏度在１０＾－９至１０＾－１１ｍｏｌ，能满足环境和食吕分析的要求。     

Measurements of nitrogen isotope composition of plants and surface soils along the altitudinal transect of the eastern slope of Mount Gongga in southwest China

The natural abundances of stable nitrogen isotopes in plants and soils have been viewed as recorders that can be used to reconstruct paleoclimate and ecological processes or to indicate the biogeochemical cycle of nitrogen in nature. This study systematically measured the nitrogen isotope composition (δ¹⁵N) in plants and surface soils along an altitudinal transect of elevation range of 1200 to 4500 m on the eastern slope of Mount Gongga in southwest China. The influences of photosynthetic pathways on plant δ¹⁵N as well as the effects of temperature and precipitation on δ¹⁵N altitudinal trends in plants and surface soils are discussed. Across this altitude transect, the δ¹⁵N values of C₃ and C₄ plants on Mount Gongga range between ?9.87‰ and 7.58‰ with a mean value of ?1.33‰, and between ?3.98‰ and 4.38‰ with a mean value of ?0.25‰, respectively. There is an evident δ¹⁵N difference between C₃ plants and C₄ plants. If, however, you only compare C₄ plants with those C₃ plants growing at the same altitudinal range, no significant difference in δ¹⁵N exists between them, suggesting that photosynthetic pathway does not have an influence on the plant δ¹⁵N values. In addition, we found that C₃, C₄ plants and surface soil (0–5 cm depth) all trend significantly towards more negative δ¹⁵N with increasing elevation. Furthermore, this study shows that the mean annual temperature and the mean annual precipitation positively and negatively correlate with δ¹⁵N in C₃ and C₄ plants, respectively. This indicates that precipitation and temperature are the main controlling factors of the δ¹⁵N variation in plants with altitude. We propose that lower δ¹⁵N values of plants and soils at higher altitude should be attributed to lower mineralization and lower net nitrification rates induced by low temperature and abundant rainfall. Copyright © 2010 John Wiley & Sons, Ltd.     

Preparative isolation and purification of ginsenosides Rf,Re, Rd and Rb1 from the roots of Panax ginseng with a salt/containing solvent system and flow step-gradient by high performance counter-current chromatography coupled with an evaporative light scattering detector

Ginseng is a popular herb worldwide and has had varied uses in traditional Asian medicine for thousands of years. There are several different species of the herb, but all share the same constituents. Ginsenosides, the most extensively studied chemical components of ginseng, are generally considered to be one of the most important active ingredients of the plant. In this study, we have developed fast and efficient methodology for isolation of four known ginsenosides Rf, Rd, Re and Rb1 from Ginseng by high performance counter-current chromatography (HPCCC) coupled with evaporative light scattering detection (ELSD). The crude sample for HPCCC was purified firstly from a ginseng extraction using macroporous resin. The enriched saponin fraction (480 mg) was separated by using methylene chloride–methanol–5 mM aqueous ammonium acetate–isopropanol (6:2:4:3, v/v,) as the two-phase solvent system and yielded 10.7 mg of Rf, 11.0 mg of Rd, 13.4 mg of Re and 13.9 mg of Rb1. The purity of these ginsenosides was 99.2%, 88.3%, 93.7% and 91.8%, respectively assessed by HPLC-DAD-ELSD, and their structures were characterized by electrospray ionization mass spectrometry (ESI-MS) and compared with standards. Ammonium acetate was used to shorten the separation time and eliminate emulsification together with a flow step-gradient. The salt can be removed by re-dissolving the sample using acetone.     

Protection against DNA damage and inhibition of lipid peroxidation by flavones from Eremosparton songoricum (Litv) Vass

Seven flavonoids were isolated from Eremosparton songoricum (Litv) Vass and their antioxidation actions were examined. To investigate protective ability against DNA damage induced by H₂O₂, human peripheral blood mononuclear cells (PBMCs) were incubated with 5-hydroxy-7,4′-dimethoxyflavone,5,7-dihydroxy-3′,4′-dimethoxyflavone, acacetin, chrysoeriol, pedalitin, flavogadorinin and 5,7,4′-trihydroxy-3′-methoxyflavone-4′-O-D-glucoside separately and then treated by H₂O₂. The percentage of damaged cells were determined by single-cell gel electrophoresis. To examine their inhibition of lipid peroxidation, the compounds were incubated with rat microsomes and the reaction was initiated by Fe²⁺/Vc. The lipid peroxidation product thiobarbituric acid reactive substances (TBARS) was determined. The result showed most of flavonoids had concentration-dependent antioxdative activities. The relationship of antioxidation and the structure is discussed.     

Carbon nanotubes as separation carrier in capillary electrophoresis

The utility and versatility of carboxylic single-walled carbon nanotubes (c-SWNT) in capillary electrophoresis (CE) is demonstrated, using as model solutes homologues and structural isomers. In the case of homologues of caffeine and theobromine, distinct changes in the electrophoretic parameters occur at a critical concentration of c-SWNT in the run buffer. It is suggested that the c-SWNT of a definite concentration could form a network in the run buffer as a pseudostationary phase on the basis of the unique tubule structure, providing a different separation from sodium dodecyl sulfate (SDS) micelles. In the case of structural isomers of catechol and hydroquinone, differing from the homologues, it is mainly attributable to the functional groups on the c-SWNT that have an effect on the electrophoretic behaviors by forming intermolecular hydrogen bonding with analytes. Furthermore, aggregated c-SWNT serve as anticonvective media and minimize solute diffusion contributing to zone broadening. The presence of charged c-SWNT suppressed the electrodiffusion and decreased the adsorption between capillary wall and solutes, which led to better peak shapes of isomers.     

纳米药物分析

介绍了纳米药物的定义,简明叙述了纳米药物的特点,探讨了新纳米药物目前研究重点,包括新纳米材料的药用功效研究、新药物载体和药物新剂型的开发及其涉及到的分析技术。展望了纳米药物对分析化学所提出的机遇和挑战。     

中国小型猪骨髓间充质干细胞的蛋白质组研究

报道了骨髓间充质干细胞(MSCs)的蛋白质组表达研究。从体外培养的MSCs提取细胞蛋白,经二维电泳分离后用银染方法可检出蛋白点约1600个,选取48个蛋白点进行胶内酶解及质谱分析,经数据库检索成功鉴定了37个蛋白,并对蛋白功能进行初步分析。本实验数据为进一步分析MSCs增殖、分化或凋亡的分子机理提供相关信息。     

A new method for stress analysis of a cyclically symmetric structure

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蓝色圆珠笔字迹色痕傅里叶变换显微红外光谱法的无损分析

利用傅里叶变换显微红外光谱法中的微区衰减全反射采样技术无损测定了纸张上圆珠笔油墨所形成的字迹色痕,获得了１０种不同圆珠笔字迹的显微红外光谱图。结果表明,笔迹色痕的微区衰减全反射谱图可明显地识别色料和溶剂的结构组成;快速地分辨各生产厂家油墨的差异。同时,纸张的不同,字迹书写的深浅均可快速,准确地进行无损分析。     

清开灵注射液HPLC/ELSD指纹图谱建立及质量相关性研究

运用高效液相色谱／蒸发光散射检测器(HPLC／ELSD)建立了复方清开灵注射液的指纹图谱。对其中7种有效成分进行了定量测定,方法学考察结果良好;通过指纹图谱相似度评价软件,对10批清开灵注射液的HPLC／ELSD指纹图谱进行了相似度计算,结果表明：10批样品相似度很好。该方法为中药质量控制提供了一种可以同时实现整体定性、指标成分定量且简便易行的方法模式。