仙茅素A的全合成

首次报道了仙茅素A[2,5-双(3,4-二羟基苯基)呋喃-3-甲醛]的全合成。以3,4-二甲氧基苯乙酮为起始原料,经Paal-Knorr反应,选择性溴代及还原等反应合成了仙茅素A,其结构经1H NMR,13C NMR和ESI-MS表征。     

复伞银莲花中的三萜皂甙

首次对复伞银莲花(AnemonetetrasepalaRoyle)全草的化学成分进行研究,从其甲醇提取物中分离出8个三萜皂甙。其中1为新化合物,命名为复伞银莲花甙(Tetrasepaloside)。根据各种波谱分析并结合化学降解将其鉴定为23-O-(2',3'-缩丙酮)-α-呋喃核糖基-常春藤配基-28-O-α-吡喃鼠李糖(1→4)-β-吡喃葡萄糖(1→6)-β-吡喃葡萄糖甙;其它7个已知化合物分别鉴定为齐墩果酸-3-O-β-吡喃葡萄糖(1→2)-α-L吡喃阿伯糖甙(2)、HN-SaponinF(3)、白头翁皂甙C(4)、木通皂甙D(5)、红毛七皂甙D(6)、刺五加皂甙A1(7)和红毛七皂甙F(8)。     

高效分离糖及糖和糖甙的α-、β-差向异构体的新型柱——β-环糊精化学键合相柱

]β-环糊精化学键合相色谱柱用于分离糖、糖醇,糖与糖甙的α-和β-差向异构体有好的分离效果。在室温,常规洗脱分离糖,大多数不存在差向异构体的分离。分离一些糖的差向异构体,在0℃有更好的效果。多种溶剂体系,如乙腈/水、丙酮/水,乙酸乙酯/甲醇/水、乙醇/正己烷等都可有好的分离效果。所有的分离都为正相体系。柱效和柱的稳定性均很好。如果使用uv检测器的低波长端（如195nm,以乙腈/水为移动相,不仅可用之检测糖,还可作梯度洗脱。     

环肽配糖体的二维核磁共振谱研究

用600MHz超导核磁共振仪测定了两个具有抗癌活性环肽配糖体RY-2和RY-3的TOCSY, HMQC, HMBC和ROESY谱图, 并正确地对分子RY-2和RY-3的氢谱和碳谱进行了归属。同时订正分子RY-3中糖的连接位置。     

制备型高效液相色谱法从积雪草提取物中分离纯化积雪草甙和羟基积雪草甙对照品

积雪草甙和羟基积雪草甙是积雪草及其相关制品质量控制的两个指标成分,本研究利用制备型高效液相色谱从积雪草提取物中同 时分离纯化得到这两个成分。对制备色谱的流动相组成、流速、进样量和检测波长等制备参数进行了优化。采用的色谱柱为C18柱(50 mm×200 mm,5 μm);流动相为甲醇-水(体积比为60∶40),流速100 mL/min;二极管阵列检测器在220 nm检测;进样体积为1.5 mL。在20 min的运行时间内,积雪草甙和羟基积雪草甙与干扰成分得到很好的分离,产品纯度达到98%以上。此方法具有快速高效、产品纯度高的 特点,可以用于制备积雪草甙和羟基积雪草甙对照品。     

蒺藜草中一个新的六糖甾体皂甙结构的NMR研究

从蒺藜草中分离得到一个新的六糖甾体皂甙，利用NMR方法，特别是2D NMR技术，确定了它的化学结构3－O－{β-D－吡喃木糖基－（1→3)-[β-D吡喃木基－（1→2)]β-D－吡喃葡萄糖甙－（1→4）－[α-L吡喃鼠李糖基－（1→2）]－β-D吡喃半乳糖基}－22－甲氧基－26－O{β-D－吡喃和葡萄糖基}－蒺藜皂甙元。     

反相液相色谱法制备纯化柠檬苦素类似物配糖体

 利用反相制备液相色谱结合吸附树脂柱色谱和离子交换色谱方法 ,从甜橙种子的提取物中纯化制备了一种柠檬苦素类似物配糖体 ,经 NMR测定为奥巴叩酮配糖体。     

胶束毛细管电泳法测定牡丹皮及芍药中牡丹酚和芍药甙

用胶束毛细管电泳地（ＭＥＣＣ）测定牡丹皮、白芍、赤芍及其不同炮制品的牡丹酚、芍药甙的含量,以３０ｍｍｏｌ／Ｌ磷酸盐缓冲溶液（ＮａＨ２ＰＯ４－Ｎａ２ＨＰＯ４）中含２０ｍｍｏｌ／Ｌ十二烷基硫酸钠（ＳＤＳ）的表面活性剂电解质,ＰＨ＝６．８５,于２５４ｎｍ紫外检测,实验结果线性关系良好。塔数达到４．６×１０＾４。     

TRITERPENE GLYCOSIDES FROM Tetrapanax papyriferum. III. MINOR MONODESMOSIDE GLYCOSIDES FROM STEM BARK

Minor monodesmoside triterpene glycosides St-A, St-B, St-C ₁ , St-D ₁ , St-C ₂ , and St-D ₂ were isolated from stem bark ofTetrapanax papyriferumC. Koch (Araliaceae). The structures of oleanolic and echinocystic acid 3-O--L-arabinopyranosides, oleanolic and echinocystic acid 3-O--D-glucopyranosyl-(13)-O--L-arabinopyranosides, and oleanolic and echinocystic acid 3-O--D-galactopyranosyl-(12)-O--L-arabinopyranosides, respectively, were proposed. Glycosides St-C ₂ , St-D ₁ , and St-D ₂ are new triterpene glycosides. The structures of the isolated compounds were established using chemical methods and NMR spectroscopy.     

STUDIES ON GLYCOSIDES ⅤⅢ.TOTAL SYNTHESIS OF NEW ALKALOID GLYCOSIDES FROM SELAGINELLA DOEDERIENII

Two new alkaloids,hordenine-O- -L-rhamnopyranoside(Ⅰ)and hordenine-0-(6′-trans-cinnamoyl)-4′-O-β-D-glucopyranosyl- -L-rhamnopyranoside(Ⅲ)isolated from Selaginella doederleinii have been synthesized the first time.A new method,in which trifluoroacetoxyl group was used both as a good leavinggroup and a protecting group for synthesis of O-glycosides with high stereo-selectivity was reported.     

Triterpenoid Saponins from Luculia pincia Hook

Two new triterpenoid saponins, cincholic acid-3-O-β-D-xylopyranoside, 28-O-β-D-glucopyranosyl ester (I), quinovic acid28-O-β-D-glucopyranosyl ester (4), and a new phenolic glucoside, 4-[4‘‘-O-( 2‘‘, 3‘‘, 5‘‘, 6‘‘-tetrahydroxy phenyl)-β-D-glucoside]-l-butene (2), along with five known triterpenoid saponins and one phenolic glucoside were isolated from the n-butanol fraction of the stems of Luculia pinciana Hook. Their structures were established by means of spectroscopic methods.     

积雪草酸衍生物的合成及抗肿瘤活性研究

以天然产物积雪草酸为起始原料,对其C-2、C-3、C-23位羟基、C-11位氢、C-28位羧基进行结构改造,合成了13个新的积雪草酸衍生物,其结构经MS及1H NMR等确证。采用MTT法,选用高表达人癌细胞(He La、Hep G2和BGC-823)对它们进行初步的体外抗肿瘤活性研究,结果表明,所测化合物对He La、Hep G2和BGC-823肿瘤细胞的抑制活性均明显强于积雪草酸,其中化合物I4和II4对He La、Hep G2和BGC-823细胞表现出很强的抑制活性,明显高于已上市药物吉非替尼,值得进一步研究。     

STEROID-SAPONINS FROM FENUGREEK SEEDS: EXTRACTION,PURIFICATION AND SURFACE PROPERTIES

Two techniques for extraction and purification were excersized in order to obtain a purified saponins extract from several sources (fenugreek, soybean, locust bean and sesame). The results indicate that fenugreek steroid saponins extract has the best surface properties and reduces the surface tension to 33.3 mN/m and the tetradecane-water interfacial tension from 44 mN/m to 7.5 mN/m. The HLB value was evaluated and found to be 18. Three different types of oil (n-tetradecane, soybean oil, tricaprylin) were emulsified with a 6 wt% aqueous solution of saponins to give an average droplet size of 0.7 μm (yet stable after month). An effective synergism is seen when these emulsions were prepared with sucrose fatty acid esters as co-surfactant. Furthermore, the foaming power was evaluated.     

Simultaneous determination of tanshinol,protocatechuic aldehyde,protocatechuic acid,notoginsenoside R1, ginsenoside Rg1 and Rb1 in rat plasma by LC–MS/MS and its application

Dantonic pill, consisting of Salviae miltiorrhize , Panax notoginseng and Borneol , is a widely used compound Chinese medicine for preventing and treating ischemic cardiovascular diseases in China. In the present study, an original and sensitive method for simultaneous determination of tanshinol (i.e. danshensu), protocatechuic aldehyde, protocatechuic acid, notoginsenoside R1, ginsenoside Rg1 and Rb1 in rat plasma by liquid chromatography–tandem mass spectrometry operated in positive/negative ion switching mode was established and validated. The lower limits of quantification for tanshinol, protocatechuic aldehyde, protocatechuic acid, notoginsenoside R1, ginsenoside Rg1 and Rb1 were 5, 0.5, 1, 0.5, 0.5 and 2 ng/mL, respectively. All of the calibration curves showed good linearity over the investigated concentration range (r > 0.99). Validation results demonstrated that the above compounds were accurately, precisely and robustly quantified in rat plasma. The method was successfully applied to characterize the pharmacokinetic profiles of all six compounds in rats following a single oral administration of Dantonic pill.     

LYOTROPIC LIQUID CRYSTALS IN BINARY SYSTEMS N-ALKYL GLYCOSIDES/WATER*

The formation of lyotropic mesophases (liquid crystals) in four binary systems n-alkyl glycosides/water was examined in dependence on surfactant concentration, temperature and the chain lengths (alkyl = heptyl, octyl, nonyl, decyl). The binary phase diagrams were established and the enthalpies of phase transitions were measured. The following phase transitions were detected by texture observation and calorimetry: hexagonal phase H, lamellar phase L, cubic phase Q, gel phase G and crystalline phase C. The positions of the corresponding regions of these phases in the phase diagram were determined. Sequence of phases and the localization of the phase regions were depended on the chain length of the alkyl group. So in the binary system n-decyl-β-D-glucoside/water the H-phase was not observed.     

HESI-MS/MS Analysis of Phenolic Compounds from Calendula aegyptiaca Fruits Extracts and Evaluation of Their Antioxidant Activities

Considering medicinal plants as an inexhaustible source of active ingredients that may be easily isolated using simple and inexpensive techniques, phytotherapy is becoming increasingly popular. Various experimental approaches and analytical methods have been used to demonstrate that the genus Calendula (Asteraceae) has a particular richness in active ingredients, especially phenolic compounds, which justifies the growing interest in scientific studies on this genus’ species. From a chemical and biological viewpoint, Calendula aegyptiaca is a little-studied plant. For the first time, high-performance liquid chromatography combined with negative electrospray ionization mass spectrometry (HPLC-HESI-MS) was used to analyze methanolic extracts of Calendula aegyptiaca (C. aegyptiaca) fruits. Thirty-five molecules were identified. Flavonoids (47.87%), phenolic acids (5.18%), and saponins (6.47%) formed the majority of these chemicals. Rutin, caffeic acid hexoside, and Soyasaponin βg’ were the most abundant molecules in the fruit methanolic extract, accounting for 17.49% of total flavonoids, 2.32 % of total phenolic acids, and 0.95% of total saponins, respectively. The antioxidant activity of the fruit extracts of C. aegyptiaca was investigated using FRAP, TAC, and DPPH as well as flavonoids and total phenols content. Because the phenolic components were more extractable using polar solvents, the antioxidant activity of the methanolic extract was found to be higher than that of the dichloromethane and hexane extracts. The IC50 value for DPPH of methanolic extract was found to be 0.041 mg·mL⁻¹. Our findings showed that C. aegyptiaca is an important source of physiologically active compounds.     

PYR树脂对甜菊糖的吸附与洗脱性能研究

系统研究了PYR型树脂对甜菊糖的吸附与洗脱性能，并与目前国内应用于甜菊糖提取分离的某些商品化吸附树脂进行了比较。结果表明，PYR树脂比其它树脂具有更优的性能，其静态吸附容量比AB—8树脂提高25％，且吸附速度快，易于洗脱再生，是一种具有工业化应用前景的新型吸附剂。     

THE SYNTHESIS AND CHARACTERIZATION OFSOME POROUS RESINS AND THEIR ADSORPTIONPROPERTY ON STEVIA GLYCOSIDES

1.INTRODUCTIONFromtheleavesofSteviaRebaudianaBertoni,asweetherbindigenoustoelevatedterrainonthebordersofBrazilandParaguay,eightsteviaglycosideshasbeenisolatedinayieldof10~15%andutilizedasahigh-sweetness,low-calorie,nonnutritionsweetener[1-3].Stevioside,rebaudiosideAandrebaudiosideCarepresentinthelargestquantitiesoftheeightsteviaglycosides.Amongthesethreeglycosides,rebaudiosideAisknownasthebestsweetenerwithrespecttotheintensityofsweetnessaswellasthequalityoftaSte,whiletheothertwomajorsw…