太空育种射干的FTIR分析

对我国首创的第4代太空育种射干与地面组射干的非晶成分从整体上进行了测定和对比分析,以期为更全面地了解太空射干品质的变化和深入研究积累资料,探索建立太空射干质量标准。结果表明两组样品的FTIR谱的主要吸收峰的峰位、峰形大致相同,但峰的强度却有明显差异。与地面组相比,太空射干在1 642 cm-1处酮类的CO伸缩振动峰增强,表明太空射干中的主要活性成分异黄酮类化合物含量明显增加,在1 318 cm-1处一水草酸钙吸收峰增加,在1 541,1 456 cm-1处分子中苯环的环伸缩振动峰、1 417 cm-1处亚甲基的C—H键弯曲振动峰以及1 051 cm-1处伯醇的C—O的伸缩振动峰都明显减弱。太空诱变育种有利于筛选出活性成分含量提高的射干新品种。预期太空射干的药效比地面组的有所增强,有待于深入研究来证实。     

A sensitive HPLC–MS/MS method for the simultaneous determination of anemoside B4, anemoside A3 and 23‐hydroxybetulinic acid: Application to the pharmacokinetics and liver distribution of Pulsatilla chinensis saponins

Pulsatilla chinensis saponins, the major active components in the herb, have drawn great attention as potential hepatitis B virus infection and hepatoma treatments. Here, a sensitive and accurate HPLC–MS/MS method was established for simultaneous determination of three saponins – anemoside B4, anemoside A3 and 23‐hydroxybetulinic acid – in rat plasma and liver, and fully validated. The method was successfully applied to a pharmacokinetics and liver distribution study of P. chinensis saponins. Consequently, 23‐hydroxybetulinic acid, with an extremely low content in the P. chinensis saponins, exhibited the highest exposure in the liver and in sites before and after hepatic disposition, namely, in the portal vein plasma and systemic plasma, followed by anemoside B4, which showed the highest content in the herb, whereas anemoside A3 displayed quite limited exposure. The hepatic first‐pass effects were 71% for 23‐hydroxybetulinic acid, 27% for anemoside B4 and 37% for anemoside A3, corresponding to their different extents of liver distribution. To our knowledge, this is the first investigation on the liver first‐pass effect and distribution of P. chinensis saponins to date. These results also provide valuable information for the understanding of the pharmacological effect of P. chinensis saponins on liver diseases.     

Simultaneous determination of 12 active components in the roots of Pulsatilla chinensis using tissue‐smashing extraction with liquid chromatography and mass spectrometry

Ultra high performance liquid chromatography coupled with mass spectrometry and combining a tissue‐smashing extraction technique was developed for the simultaneous quantitative analysis of 12 compounds in the roots of Pulsatilla chinensis . Among them, compound 6 was characterized and accurately quantified in this herb for the first time. The parameters of extraction condition were simultaneously optimized with a Box–Behnken design and Derringer's function. The optimized conditions were as follows: sample quantity of 0.5 g, ethanol concentration of 70%, and extraction time of 200 s. Multiple‐reaction monitoring scanning was employed for the quantification between positive and negative mode in a single run of 6 min. Full validation of the method was carried out, and the results indicated that the method was rapid, specific, and reliable. The developed method was successfully applied to quantify the 12 compounds in 33 batches of P. chinensis from different provinces. Moreover, the principal component analysis was performed to compare the P. chinensis collected from different provinces of China based on quantitative data and the results indicated that the content of compounds could be used to differentiate the origins of P. chinensis . These results demonstrated that this method is feasible and reliable for the quality control of P. chinensis .     

夏蜡梅果实和种子形态变异及其与环境因子相关性

对天台大雷山4个不同生境（常绿阔叶林、灌丛、竹林和杉木林）夏蜡梅群体的果实、种子形态变异及其与环境因子的相关性进行了研究．测量的果实和种子12项形态学指标表明,果实和种子的性状以灌丛生境最优、其次是竹林生境、最差的是常绿阔叶林生境．表型性状在群体间和群体内都存在着一定程度的变异,其中群体间的变异系数的平均值从61．71（每果种子数）到7．51（种子厚）．夏蜡梅种子形态较果实形态稳定．单因素方差分析显示．夏蜡梅果实和种子形态在不同生境间差异显著,其中80％以上的变异来源于生境内．PCA分析结果将4个群体大致分为3组,杉木林生境和常绿阔叶林生境果实和种子形态最接近,为一组,竹林生境和灌丛生境各为一组．夏蜡梅果实和种子形态与光照条件的相关性最大,与土壤因子的相关性较小．     

Microwave-assisted extraction and fingerprint studies of Schisandra chinensis (Turcz.) by high performance liquid chromatography and gas chromatography

In order to choose an appropriate extraction method, samples of Schisandra chinensis (Turcz.) Baill were extracted by different methods and it was found that microwave-assisted extraction gave the best results. The contents of schisandrin, schisantherin, deoxyschizandrin, and r-schizandrin of 10 samples collected from different regions in China were determined by HPLC. The chromatograms of ten samples were used to establish the fingerprints of Schisandra chinensis (Turcz.) Baill and two methods based on HPLC and GC were applied to them simultaneously. The fingerprints consisted of 18 common peaks obtained by HPLC and 17 common peaks obtained by GC, which showed good stability and repeatability with RSD less than 3% for retention time. The fingerprints are suitable for identifying and differentiating samples by geographical origin and can be used for quality control.     

Separation and purification of 9,10‐dihydrophenanthrenes and bibenzyls from Pholidota chinensis by high‐speed countercurrent chromatography

Stilbenoids are the main components of leaves and stems of Pholidota chinensis. In the present investigation, high‐speed counter‐current chromatography was used for the separation and purification of two classes of stilbenoids, namely, bibenzyls and 9,10‐dihydrophenanthrenes, on a preparative scale from whole plants of P. chinensis with different solvent systems after silica gel column chromatography fractionation. n‐Hexane/ethyl acetate/methanol/water (1.2:1:1:0.8, v/v/v/v) was selected as the optimum solvent system to purify 1‐(3,4,5‐trimethoxyphenyl)‐1′,2′‐ethanediol ( 1 ), coelonin ( 2 ), 3,4′‐dihydroxy‐5,5′‐dimethoxybibenzyl ( 3 ), and 2,?7‐?dihydroxy‐?3,?4,?6‐?trimethoxy‐?9,?10‐?dihydrophenanthrene ( 4 ). While 2,7‐dihydroxy‐3,4,6‐trimethoxy‐?9,?10‐?dihydrophenanthrene ( 5 ), batatasin III ( 6 ), orchinol ( 7 ), and 3′‐O‐methylbatatasin III ( 8 ) were purified by n‐hexane/ethyl acetate/methanol/water (1.6:0.8:1.2:0.4, v/v/v/v). After the high‐speed counter‐current chromatography isolation procedure, the purity of all compounds was over 94% assayed by ultra high performance liquid chromatography. The chemical structure identification of all compounds was carried out by mass spectrometry and ¹H and ¹³C NMR spectroscopy. To the best of our knowledge, the current investigation is the first study for the separation and purification of bibenzyls and 9,10‐dihydrophenanthrenes by high‐speed counter‐current chromatography from natural resources.     

Complete NMR spectral assignments of two new iridoid diastereoisomers from the flowers of Plumeria rubra L. cv. acutifolia

Two new iridoid diastereoisomers (1, 2), together with five known compounds, were isolated from the flowers of Plumerian rubra L. cv. acutifolia. Their structures were elucidated by the means of in-depth spectroscopic and mass-spectrometric analyses, particularly 1D and 2D NMR spectroscopy.     

五味子治疗大鼠糖尿病肾病作用机制的血清代谢组学研究

采用基于超高效液相色谱与串联四级杆飞行时间质谱仪(Ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry,UPLC/Q-TOF-MS)联用技术的代谢组学方法,通过分析大鼠血清内源性代谢物的变化,研究五味子治疗糖尿病肾病的作用机制。利用高脂高糖饲料喂养并腹腔注射链脲佐菌素(STZ)建立糖尿病大鼠模型。给药12周后,采用试剂盒方法测定尿蛋白、尿肌酐的含量,结果表明五味子水提取物可以显著降低模型动物的尿蛋白含量(p<0.05),对糖尿病大鼠肾病并发症具有一定的改善作用。采用UPLC/Q-TOF-MS方法分析了五味子对糖尿病肾病大鼠的血清代谢轮廓,分析了健康组、模型组和五味子给药组的大鼠血清,采用偏最小二乘法-判别分析(Partial least squares discriminant analysis,PLS-DA)进行数据分析。PLS-DA得分图显示健康组、模型组和五味子组的代谢轮廓有显著差别,根据正交偏最小二乘法-判别分析(Orthogonal partial least squares discriminant analysis,OPLS-DA)载荷图筛选,将对各组分离贡献大的化合物的串联质谱分析数据,经Human Metabolome Database(HMDB)等数据库检索,进行质谱信息匹配,鉴定出黄尿酸、油酰胺、棕榈酰胺、尿酸、5-羟基己酸、硫酸对甲酚、对甲酚葡萄糖苷酸7种内源性代谢物为生物标记物。研究结果表明五味子通过影响色氨酸代谢、嘌呤代谢、肠内菌代谢、脂肪酸代谢等通路对糖尿病肾病发挥治疗作用,其中嘌呤代谢、肠内菌代谢通路可能是五味子发挥治疗作用的重要途径。     

A Furostanol Saponin from the Cytotoxic Fraction of Tupistra chinensis Rhizomes

More than 1800 species of medicinal plants grow in Shennongjia Forest District. Most of them were recorded to be used as anti-inflammatory agents in the folk medicine1. Kaikoujian, a Chinese name for rhizomes of Tupistra chinensis Bak., is a reputed folk …     

加速溶剂萃取法快速提取黄连中的生物碱

探讨了快速溶剂萃取法（ASE）提取黄连中生物碱的可行性,并比较了该方法与回流提取法和超声提取法的优越性。以黄连中盐酸小檗碱的提取率为指标,以高效液相色谱法（HPLC）为检测方法,用正交实验对快速溶剂萃取法从黄连中提取盐酸小檗碱的工作条件进行优化。最佳仪器参数：提取溶剂为80%乙醇＋0.5%HCl,提取温度为130℃,静态提取时间为10 min,提取次数为1次。快速溶剂萃取法可作为黄连中生物碱分析测定的前处理方法。