PB实验设计联用CCD-RSM优化虎眼万年青多糖铁复合物的制备工艺

为了探究虎眼万年青多糖铁(Ⅲ)复合物(OPIC)的最佳合成方法,我们采用Plackett-Burman设计对虎眼万年青多糖铁复合物制备工艺的主要影响因素进行考察,联用星点设计(central composite design,CCD)效应面法对显著性因素的水平进行优化,以溶剂加入量、三氯化铁加入量、多糖和柠檬酸钠加入量的比例、温度以及pH值为自变量,以虎眼万年青多糖铁中铁含量为因变量,通过对自变量与因变量的完全二次响应曲面的回归拟合,用效应面法预测最佳工艺.结果表明:温度、pH值和质量比对虎眼万年青多糖铁的合成有显著性意义;二项式方程拟合度高,相关系数r=0.987 9.虎眼万年青多糖铁的最佳合成工艺:溶剂的加入量为70mL,三氯化铁的加入量为6mL,温度80℃,质量比为3.5,pH值为8.最终利用PlackettBurman实验设计连用CCD确定了虎眼万年青多糖铁的最佳合成工艺,该方法简便,预测性好,重现性高.     

一个新倍半萜内酯的分离与结构研究

自蒿属植物万年蒿(Artemisia sacrorumLedeb)地上部分分离得三个倍半萜内酯类化合物,经理化常数测定,化学相关及光谱(红外光谱1、H-核磁共振光谱1、3C-核磁共振光谱、质谱)分析,鉴定其结构分别为万年蒿氯内酯chlorosacroratin(Ⅰ),去乙酰氧母菊内酯deacetoxymatricarin(Ⅱ)和ridentin(Ⅲ)。其中,万年蒿氯内酯为一未见报道的新化合物。     

紫玉盘种子中的番荔枝内酯成分研究 Ⅰ.紫玉盘素(Microcarpacin)的分离及结构鉴定

从紫玉盘(Uvaria microcarpa Champ.ex Benth)种子中首次分离得到一个新的邻双四氢呋喃环番荔枝内酯(Annonaceous acetogenin)化合物—紫玉盘素(Microcarpacin).同时首次以纯化合物形式分离得到两个已知的番荔枝内酯NarumicinsⅠ和Narumicins Ⅱ.     

紫玉盘种子中的番荔枝内酯成分研究I. 紫玉盘素(Microcarpacin)的分离及结构鉴定

从紫玉盘(Uvaria microcarpa Champ. ex Benth)种子中首次分离得到一个新的邻双四氢呋喃环番荔枝内酯(Annonaceousacetogenin)化合物-紫玉盘素(Microcarpacin)。同时首次以纯化合物形式分离得到两个已知的番荔枝内酯Narumicins I和Narumicins II.     

紫玉盘种子中的番荔枝内酯成分研究I. 紫玉盘素(Microcarpacin)的分离及结构鉴定

从紫玉盘(Uvaria microcarpa Champ. ex Benth)种子中首次分离得到一个新的邻双四氢呋喃环番荔枝内酯(Annonaceousacetogenin)化合物-紫玉盘素(Microcarpacin)。同时首次以纯化合物形式分离得到两个已知的番荔枝内酯Narumicins I和Narumicins II.     

线叶紫菀中一个单萜酸的化学结构

线叶紫菀中一个单萜酸的化学结构王明安，陈耀祖（北京农业大学应用化学系，北京，１０００９４）（兰州大学化学系）关键词线叶紫菀，单萜，结构分析线叶紫菀（ＡｓｔｅｒｆａｒｒｅｒｉＷ．Ｗ．ＳｍｉｔｈｅｔＪ．Ｆ．Ｊｅｆｆｅｒｙ）系菊科紫菀属多年生草本植物，用于...     

生姜内酯的分离与结构表征

从荜澄茄药材粗粉中分离得生姜内酯晶体(1),其结构经NMR和X-射线单晶衍射分析确证。1的晶体为单斜晶系,空间群P21/c,晶胞参数a=8.780 9(5),b=19.923 9(9),c=7.139 1(4),β=107.299(6)°,V=1 192.49(10)3,Z=4,F(000)=512.0,R1=0.049 3,wR2=0.109 4。1为首次从樟科植物中发现,由于其具有罕见的三环骈双内酯结构,其完整的结构表征对类似化合物的结构鉴定具有重要的参考价值。     

双表白术内酯的结构鉴定

白术(ArtactylodesmacrocephalaKoidz)为有多种生物活性的传统常用中药。从中分得4个已知化合物,另外一个物质的MS,1D和2DNMR表明是类型较为罕见的完全对称的双倍半萜新化合物,命名为双表白术内酯(biepiasterolid)。     

麝香草的新单萜配糖物的分离与合成

从麝香草(Thymus vulgaris L)的甲醇萃取物中分离出三个单萜配糖物. 用核磁共振光谱确定了它们的结构为对伞花-9-基-β-D-葡糖苷(1), 5-β-D-葡糖苷百里氢醌(2)和2-β-D-葡糖苷百里氢醌(3). 其中1是新化合物, 用以对伞花-9-醇为原料的对映体选择性合成方法确定了化合物1的8位的立体化学为R型.     

Chemical Characteristic of Bioactive Polysaccharides Isolated from Ornithogalum caudatum Ait.

A water-soluble crude extract prepared from Ornithogalum caudatum Ait. (()CA) showing a high immunomodulating activitiy was isolated and characterized by virtue of gel filtration and column chromatography. The presence of the monosaccharides has been established by the chemical analysis. The quantitative analysis of the alditol acetate derivatives of them showed the ratios of the monosaccharides analyzed by means of GC respectively. The concentrations of protein(280 nm) and carbohydrate(496 nm) were detected respectively. The information of the molecular weight from the pure polysaccharide was obtained by several standard Dextrans from the Sephadex chromatography.     

Synthesis and Crystal Structure of a Novel Lactone Derived from Dehydroabietic Acid

A novel lactone derived from dehydroabietic acid,C20H21BrO4,has been charac-terized by IR,1H NMR,13C NMR and single-crystal X-ray diffraction method.It crystallizes in orthorhombic,space group P212121 with a = 6.4195(15),b = 11.535(3),c = 24.654(6) ,V = 1825.5(7) 3,Z = 4,Mr = 405.28,Dc = 1.475 g/cm3,λ = 0.71075 ,μ(MoKα) = 2.27 mm-1,F(000) = 832,the final R = 0.024 and wR = 0.045 for 2152 observed reflections with I 2σ(I).The molecules of lactone are mainly linked through intermolecular hydrogen bonds.     

朝鲜淫羊藿中生物碱类新成分的分离提取及结构鉴定

淫羊藿系小檗科淫羊藿属植物 ,具有补肾壮阳、强筋骨、祛风湿之功效 .现代药理研究表明 ,它还具有防治骨质疏松和提高免疫功能等作用 .2 0 0 0年版中国药典收载了 5种淫羊藿属植物 ,朝鲜淫羊藿为其中一种 ,是长白山道地中药材之一 .朝鲜淫羊藿中化学成分的研究多集中在黄酮类化合物方面 [1～ 6 ] ,而对其生物碱类化合物的研究较少 [7,8] .本文对朝鲜淫羊藿中生物碱类化合物进行了研究 ,并发现了一种新的生物碱 (6-羟基 -1 1 ,1 2 -二甲氧基 -2 ,2 -二甲基 -1 ,8-二氧 -1 ,3 ,4,8-四氢 -2 H -7-氧杂 -2 -氮 -苯并 [c]菲 ) ,采用核磁共振波…     

Isolation and Identification of Novel Compounds from Mulgedium tatarica DC.

Our study focused on the chemical constituents of Mulgedium tatarica that was collected from Inner Mongolia autonomous region of China. It is not only a folk medicinal herb but also a wild vegetable. It was reported that this plant showed several bioactivities, such as diuretic action, stimulating milk secretion, analgesia and haemorrhoidolysis. [1 ] Fatty acids and other volatile components of Mulgedium tatarica were detected by GC-MS for the first time. [2] From the ethanol extract of the whole plant of Mulgedium tatarica DC., two new compounds, named tataricoside and mulgedin A, have been isolated and characterized. Their structures were identified by UV, IR,HRFABMS, 1H NMR, 13C NMR, HMQC, HMBC and 1H-1H COSY spectral analysis.     

玉米苞叶中新黄酮类化合物的分离和鉴定

从玉米(Zea mays L)苞叶乙醇提取物中分离得到了4个黄酮类化合物, 采用UV, IR, MS, 1D NMR和2D NMR方法对化合物的结构进行了鉴定, 它们分别为苜蓿素(1)、苜蓿素-5-O-β-D-吡喃葡萄糖苷(2)、苜蓿素-7-O-β-D-吡喃葡萄糖苷(3)和苜蓿素-7-O-[β-D-呋喃芹糖基-(1→2)]β-D-吡喃葡萄糖苷(4). 其中, 化合物4为新化合物, 化合物1~3为首次从该植物中分离得到.     

软珊瑚Sarcophyton crassocaule中Cembrane型二萜的分离与鉴定

从采自中国南海西沙群岛海域的软珊瑚Sarcophytoncrassocaule中分离得到一种结构新颖的Cembrane型二萜,经¹HNMR,¹³CNMR,HMQC,¹H-¹HCOSY,NOESY,FABMS和X射线晶体衍射确定其结构,命名为SarcocrassolideB它对P388的细胞毒性为1.5μg/mL.     

Simultaneous determination of matrine, sophoridine and oxymatrine in Sophora flavescens Ait. by high performance liquid chromatography

Following a detailed study, a reversed-phase high performance liquid chromatographic method (HPLC) has been developed and validated for analysis of three bioactive alkaloids, matrine, sophoridine and oxymatrine, in Sophora flavescens Ait. HPLC separation of the alkaloids was performed on a Kromasil C(18) column and detected by ultraviolet absorbance at 208 nm. The column temperature was maintained at 40 degrees C. A mobile phase composed of 0.01 mol/L KH(2)PO(4) buffer-methanol-triethylamine in the ratios 94:6:0.01 (v/v) was found to be the most suitable for this separation at a fl ow-rate of 1.0 mL/min and enabled the baseline separation of the three analytes free from interferences with isocratic elution. The analysis time was 24 min per injection. The calibration was linear in the range of 0.2-120.0 micro g/mL for matrine, 0.2-115.2 micro g/mL for sophoridine and 0.2-110.4 micro g/mL for oxymatrine, respectively. For assaying Sophora Flavescens Ait. samples, the relative standard deviations were 2.0% for matrine, 2.8% for sophoridine and 1.8% for oxymatrine analysis. The average recoveries of matrine, sophoridine and oxymatrine were 93.9, 95.3 and 93.5% for the Sophora flavescens Ait. samples, respectively. The method has been successfully applied to the simultaneous determination of matrine, sophoridine and oxymatrine in Sophora Flavescens Ait. samples collected in different habitats.     

Novel Glycerophospholipid,Lipo- and N-acyl Amino Acids from Bacteroidetes: Isolation,Structure Elucidation and Bioactivity

The ‘core’ metabolome of the Bacteroidetes genus Chitinophaga was recently discovered to consist of only seven metabolites. A structural relationship in terms of shared lipid moieties among four of them was postulated. Here, structure elucidation and characterization via ultra-high resolution mass spectrometry (UHR-MS) and nuclear magnetic resonance (NMR) spectroscopy of those four lipids (two lipoamino acids (LAAs), two lysophosphatidylethanolamines (LPEs)), as well as several other undescribed LAAs and N-acyl amino acids (NAAAs), identified during isolation were carried out. The LAAs represent closely related analogs of the literature-known LAAs, such as the glycine-serine dipeptide lipids 430 (2) and 654. Most of the here characterized LAAs (1, 5–11) are members of a so far undescribed glycine-serine-ornithine tripeptide lipid family. Moreover, this study reports three novel NAAAs (N-(5-methyl)hexanoyl tyrosine (14) and N-(7-methyl)octanoyl tyrosine (15) or phenylalanine (16)) from Olivibacter sp. FHG000416, another Bacteroidetes strain initially selected as best in-house producer for isolation of lipid 430. Antimicrobial profiling revealed most isolated LAAs (1–3) and the two LPE ‘core’ metabolites (12, 13) active against the Gram-negative pathogen M. catarrhalis ATCC 25238 and the Gram-positive bacterium M. luteus DSM 20030. For LAA 1, additional growth inhibition activity against B. subtilis DSM 10 was observed.