Studies on the Chemical Constituents of Rhodiola fastigita S. H. Fu

Rhodiola fastigita is an alpine plant growing at 3300--5400 m above sea level. Seven crystal, compounds were isolated from the rhizome of this plant. They were identified as β- sitosterol, β-sitosterol-3-β-D-galactoside, daucosterol, gallic acid, gallic acid ethyl ester, p-tyrosol and herbacetin-8-arabinoside by IR, MS, H-NMR and chemical method. Daucosterol, β-sitosterol- 3-β-D-galactoside and gallic acid ethyl ester were obtained from the genus Rhodiola L. for the first time.     

Study on Chemical Components of Davidia involucrata Baill. Native to China

Six compounds have been isolatea from the branch of Davidia involucrata Baill which is native to China. Their structures were identified as taraxerone (D1), taraxerol (D2), β-sitoste- rol (D3), 3′-O-methyl- 3, 4-O, O-methylideneellagic acid (D4), 3, 3′, 4-5-trimethylellagic acid (D5) and ellagic acid (D6) by means of chemical methods and IR 1H-NMR, MS, respectively.     

Studies on the Chemical Constituents of the Root of Libanotis buchtorimensis Fisch Dc.

Two crystalline substances were isolated from the root of Libanotis buchtorimensis (Fisch) Dc., one of them identified as trans-P-hydroxy-cinnamic acid. It was first found in this plant, Compound (Ⅷ)is anew compound, white needle crystal, melting point 189-191℃, with the empirical formula C14H14O4, its structure was elucidate by means of UV, IR, 1H-NMR, 13C-NMR and MS, It was named libanotin A.     

High yield production of salidroside in the suspension culture of Rhodiola sachalinensis

Salidroside has been identified as the most potent ingredient of the Chinese medicine herb, Rhodiola sachalinensis. Since the natural supply of this herb is rapidly decreasing, we established a compact callus aggregate (CCA) strain and culturing system for high yield salidroside production. Several callus strains induced from the explants originated from root, stem, leaf and cotyledon of R. sachalinensis were established and screened for rapid growth rate, high salidroside content and easy propagation in suspension culture condition. The CCA strain was established from a callus strain initiated from the cotyledon. The kinetics of dry weight accumulation and cellular salidroside content in various culture conditions for the strain was determined. For high salidroside production, the optimal inoculum amount was 10% and the optimal concentration for 6-benzylaminopurine and indole-3-butyric acid added in the liquid medium was 5 and 2.5 mg l-1, respectively. The acidic culture medium and a faster shaking speed favored the salidroside accumulation. The addition of 2,4-D, in the liquid MS medium and the utilization of L-tyrosol for chemical feeding enhanced salidroside production. Using a proper combination of culture condition and treatment, salidroside accumulation could reach 57.72 mg g-1 dry weight, that was 5-10-fold higher than that detected in field-grown plants. The corresponding salidroside yield was 555.13 mg l-1, a level suitable for cost effective commercial production to compensate the natural resource shortage of R. sachalinensis.     

Studies on Neotriptetraolide Isolated from Tripterygium wilfordii Hook. f.

A new diterpenoid bisepoxide, neotriptetraolide, was isolated from the leaves and root of Tripterygium wilfordii Hook. f. Neotriptetraolide was crystallized from CH3OH as colorless needle-like crystal, with amp of 237～238 ℃. Its molecular formula was C20H2608. Its structure was elucidated by means of spectral analysis (UV, IR, MS, 1H-NMR, 13C- NMR, 2D-COSY, 2D-NOESY, 13C-NOE, and selective long-range DEPT spectroscopy) and the computation of molecular mechanics and molecular graph.     

Quantitative determination of salidroside in rat plasma by on-line solid-phase extraction integrated with high-performance liquid chromatography/electrospray ionization tandem mass spectrometry

A method for the quantification of salidroside, a major biologically active compound in Rhodiola, in rat plasma by on-line SPE LC/MS/MS in negative electrospray mode was developed and validated. A column-switching instrument and two HPLC pumping systems were employed, and salicin was used as the internal standard. A Waters Oasis HLB extraction column and an Agilent TC-C(18) analytical column in a column-switching set-up with gradient elution were utilized. The MS/MS ion transitions monitored were m/z 299.0/119.0 and 285.1/122.9 for salidroside and salicin, respectively. The standard curves were linear within a range of 50-5000 ng/mL using weighted linear regression analysis (1/x). The intra- and inter-day coefficients of variance ranged from 1% to 9%. The recovery was above 90%. The freeze/thaw and long-term stability were validated. This method was subsequently applied to a pharmacokinetic study of salidroside in rats.     

Synthesis of a water-soluble protein cross-linking reagent

2,4-Difluoro-5-nitrobenzenesulfonic acid has been synthesized by the sulfonation of 2,4-difluoronitrobenzene, and precipitated with KCl as the potassium sulfonate. The structure was confirmed by chemical and spectroscopic methods (IR, 1H-NMR, 13C-NMR, 19F-NMR, UV, MS and ultimate organic analysis). Lysozyme was cross-linked with the potassium sulfonate and with 1,5-difluoro-2,4-dinitrobenzene. The products were analysed by SDS-PAGE and compared. The cross-linking conditions were optimized.     

Studies on the Triterpenes of Terminalia chebula Retz.

Four triterpenes have been isolated from the alcoholic extract of Terminalia Chebula Retz.. Three of them have been identified as terminoic acid (T1), arjugenin (T2) and arjunolic acid(T3). T4 is a new compound, named chebupentol. Its structure was established to be olean-12-ene-2,3,19,23,28-pentol on the basis of its IR, MS, 1HNMR, 13CNMR, 1H-13C 2D NMR, 1H-1H 2D NMR and NOESY 2D NMR. The structure of compound T4 was confirmed by the chemical transformation of T4 from arjugenin (T2) with LiAlH4.     

高山红景天细胞悬浮培养中红景天甙生物合成代谢的调控 Ⅰ:前体的影响

探索了高山红景天(Rhodiola sachalinensis A.Bor)细胞培养中红景天甙生物合成的途径,认为甙元酪醇是经由莽草酸途径生成的。在此基础上研究了酪醇、L-酪氨酸与L-苯丙氨酸三种前体加入对红景天甙生物合成的调控作用。结果表明,酪醇、酪氨酸等前体易被多酚氧化酶氧化成褐色,用与前体浓度为1:1的V。来防止褐化效果显著;浓度为0.5mmol/L的酪醇,酪氨酸及苯丙氨酸在细胞培养15d时添加,使红景天甙含量由0.336％分别提高到1.43％、1.11％、0.85％。     

Studies on the Chemical Constituents from Root Bark of Aralia armata (Wall.) Seem.

Eleven constituents were isolated from root bark of Aralia armata (Wall.) Seem. Their structures were elucidated by spectra(IR, MS, 1H-NMR and 13C-NMR) and chemical analyses. They were deglucose chikusetsusaponin Ⅳ (AT–Ⅰ), chikusetsusaponin Na (AT–Ⅱ ), zingibroside R1 (AT–Ⅲ), ginsenin R0 (AT–IV), decaisneanaside (AT–Ⅴ), armatoside (AT-Ⅶ), araloside A (AT–Ⅶ), octacosanoic acid (AT–Ⅷ), β-sitosterol (ATIX ), mixture of β-sitosterol and stigmastterol (AT–×), oleanolic acid (AT–Xl ). They were for the first time found in this plant, AT–Ⅵ is a new saponin.     

A New Diterpene Glycoside in Aster ageratoides Turcz.

A new natural diterpene glycoside was isolated from Aster ageratoides Turcz. Its structure was elucidated by means of IR, MS (FAB, EI), NMR (1H-, 13C-, DEPT), 2D-NMR (1H-1H COSY, 13C-1 H COSY, J-resolved, CoLoC) spectra and chemical method as 16β, 17-dihydroxy- (—) -kauran- 19-oic acid-β-D-glucopyanosyl ester.     

Studies on the Constituents of Aristolochia versicolar S. M. Hwang

Twenty-four constituents were isolated from the root of Aristolochia versicolar S. M. Hwang (collected from Guangxi province, China). Ten of them (two novel sesquiterpene lacrones and eight known compounds) were reported recently. This paper deals with the other eight compounds. From the petroleum ether extraction a sesquiterpene lactone, C15H20O2, mp. 94–95℃ [α]D36 –49˚ (C=1.8, EtOH), confirmed to be isoaristolactone, was obtained from plants for the first time. On the basis of spectral analysis (UV, IR, 1HNMR, 13CNMR, MS) and chemical reactions its structure was determined as B2. From the petroleum enter unsoluble sec- tion 6-methoxyaristolic acid methyl ester (D1), aristolic acid (D3), 6-methoxyaristolic acid (ari- stolinic acid) (D4f), 6-methoxyaristolochic acid methyl ester (D4y), aristolochic acid A(D5), β-sitosterol-D-glucoside (D10) and allantoin (C2) were isolated and identified. Dx, Ds, and Ds show ed antifertility activity in mice.     

南海海绵Pachychalinasp.化学成份的研究

从中国南海海绵Pachychalina sp.正丁醇可溶部分获得了5个化合物,通过UV,IR,~1H-NMR,~(13)C-NMR,MS,~1H-~1HDQFCOSY等实验确定了它们的结构分别是:对羟基苯醋酸甲酯(1),胸腺嘧啶(2),尿嘧啶(3),胸腺嘧啶脱氧核苷(4)和尿嘧啶脱氧核苷(5)。其中化合物(1)是首次从我国南海海洋生物中获得;化合物(5)则是首次从海绵中分离得到的天然产物。     

Two New Buxus Alkaloids from Buxus Microphylla Sieb. et Zucc.

Five compounds were isolated from Buxus microphylla Sieb. et Zucc. Based on the physico-chemical constants and spectral analysis (IR, MS, 1H-NMR and 13C-NMR), they were identified as cycloprotobuxinamine ( Ⅰ ), buxmicrophylline A ( Ⅱ ), buxtauine M ( Ⅲ ), isoscopoletin (Ⅳ) and epi-lupeol ( Ⅴ ). ( Ⅰ ) and ( Ⅱ ) were new compounds. The structure of buxmicrophylline ( Ⅱ ) was confirmed by X-ray crystallographic analysis.     

Studies on the Naphthaquinone Constituents of Onosma confertum W. W. Smith and Quantitative Determination of Shikonin

Four compounds were isolated from Onosma confertum W. W. Smith. They were identified as deoxyshikonine (Ⅰ), β, β-dimethylacrylshkonin (Ⅱ), acetylshikonine (Ⅲ) and shikonin (Ⅳ) according to their physical and chemical constants from MS, IR, 1H-NMR, CD-HPLC determination. The total quantity of shikonin obtained after basic hydrolysis of its derivatives was determined.     

药用异喹啉生物碱的研究：Ⅱ.地不容生物碱的研究

从地不容块根中分得四种生物碱A、B、C、D,经UV,IR,~1H-NMR,~(13)C-NMR,HRMS等方法鉴定了它们的结构,分别是cepharanthine (A),1-curine (B),isochondodendrine (C),ushinsunine (D)。C,D系首次从该植物中获得。     

Structural Study of Triptriolide Isolated from Tripterygium wilfordii

A novel diterpene bisepoxide, ,riptriolide was isolated from the root and leaves of Tripterygium wilfordii Hook- f. Triptriolide was obtained as white cluster crystal, mp. 260-262℃. Its molecular formula is C20H26O7. The structure and stereochemistry of triptriolide were determined by UV, IR, MS, 1H-NMR, 13C-NMR, 2d-NMR, 13C-NOE, NOE difference spectroscopy and direct X-ray crystallographic analysis. Preliminary pharmacologic assay revealed that triptriolide has a potent anti-inflammatory action.     

Studies on the Chemical Constituents of Xylanche himalaica

Six compounds were isolated from the tuber of Xylanche himalaica (Hook. f. et Thorns.) G. Beck Based on the physico-chemical constants, spectral analysis (IR, MS, 1H-NMR, 13C-NMR)and preparation of the derivative, they were identified as 3-epi-acetoxyurs-12-en-28-al (Ⅰ), ursolic acid (Ⅱ), 3-epi-ursolic acid (Ⅲ), (+)-pinoresinol (Ⅳ), (+)-pinoresinol monoglucoside (Ⅴ) and daucosterol (Ⅵ). Ⅰis a new compound.     

产D-阿拉伯醇菌株的筛选、鉴定及其产D-阿拉伯醇条件的优化

摘要：【目的】产D-阿拉伯醇的耐高渗酵母的筛选、鉴定和产D-阿拉伯醇条件的优化。【方法】通过电镜、Biolog GN、(G+C)含量和26S rDNA D1/D2区序列分析法对所获得的菌株进行了描述。通过红外光谱、核磁共振氢谱和碳谱、质谱以及旋光度实验鉴定纯化产物的结构。通过单因素实验优化产D-阿拉伯醇的发酵条件。【结果】本文筛选得到一株产D-阿拉伯醇的新型菌株,经鉴定属于假丝酵母属并命名为Candida sp. H2。200 mL摇瓶发酵生产D-阿拉伯醇的单因素优化实验表明,最适发酵条件为：葡萄糖250     

Two Novel Diterpenoid Alkaloids Isolated from the Roots of Aconitum brevicalcaratum

Two new diterpenoid alkaloids were isolated from the roots of Aconitum brevicalcaratum Diels. They were acobretine D ( Ⅰ )and acobretine E ( Ⅱ ), and the structures of which were identified on the basis of spectroscopic evidences (IR, MS, 1 H and 13C-NMR) and confirmed by chemical transformations. The 1 H and 13C chemical shifts of the hydrochloride of Ⅰ were assigned in relation to of 1 H-1 H COSY and 13C-1 H COSY.