Determination of fifteen bioactive components in Radix et Rhizoma Salviae Miltiorrhizae by high-performance liquid chromatography with ultraviolet and mass spectrometric detection

A high-performance liquid chromatographic (HPLC) method coupled with ultraviolet (UV) and electrospray ionization time-of-flight mass spectrometry (ESI-TOF/MS) was established for simultaneous qualitative and quantitative determination of nine phenolic acids and six diterpenoids in Radix et Rhizoma Salviae Miltiorrhizae (RRSM). The optimal chromatographic conditions were achieved on a Zorbax C(18) column by gradient elution with 0.1% (v/v) aqueous formic acid and acetonitrile as mobile phase at the flow rate of 1.0 mL/min. The detection wavelength at 281 nm was chosen to determine the 15 bioactive components, namely danshensu (1), protocatechuic acid (2), protocatechuic aldehyde (3), caffeic acid (4), rosmarinic acid (5), lithospermic acid (6), salvianolic acid B (7), salvianolic acid A (8), salvianolic acid C (9); dihydrotanshinone I (10), cryptotanshinone (11), tanshinone I (12), methylene tanshiqunone (13), tanshinone IIA (14) and miltirone (15). Additionally, LC-ESI-TOF/MS was used to make definite identification of the constituents in samples in comparison with those reference compounds. The validation of the method included tests of linearity, sensitivity, repeatability, stability and recovery. The proposed method was successfully applied to quantify the 15 components in 21 samples; significant variations were demonstrated in the contents of the samples from diverse species and origins. The developed method could be used to effectively and comprehensively evaluate the quality of RRSM for its clinical safety and efficacy.     

Extension of the non-uniform warping theory to an orthotropic composite beam

This Note proposes an extension to composite section of the non-uniform (out-of-plane) warping beam theory recently established for homogeneous and isotropic beam by R. El Fatmi (C. R. Mecanique 335 (2007) 467–474). For the present work, which constitutes a first step of this extension, the cross-section is assumed to be symmetric and made by orthotropic materials; however, Poisson's effects (called here in-plane warping) are also taken into account. Closed form results are given for the structural behavior of the composite beam and for the expressions of the 3D stresses; these ones, easy to compare with 3D Saint Venant stresses, make clear the additional contribution of the new internal forces induced by the non-uniformity of the (in and out) warpings. As first numerical applications, results on torsion and shear-bending of a cantilever sandwich beam are presented.     

Valeurs d'une fonction de Picard en des points algébriques

Using geometric tools introduced by P. Cohen, H. Shiga, J. Wolfart and G. Wüstholz, we show in Theorem 1 that when a certain Gauss hypergeometric function takes an algebraic value at an algebraic point, then another Gauss hypergeometric function takes a transcendental value at a related algebraic point. Using Appell hypergeometric functions, which generalize to two variables the Gauss functions, we study values at algebraic points of a new transcendental function defined in terms of these two functions. By Theorem 2, these values correspond to abelian varieties in the same isogeny class. Using a result of Edixhoven-Yafaev [B. Edixhoven, A. Yafaev, Subvarieties of Shimura varieties, Ann. of Math. 157 (2003) 621-645], this last result is in turn related to the distribution of the moduli of such abelian varieties in certain Shimura varieties.     

Temperature-assisted ionic liquid dispersive liquid-liquid microextraction combined with high performance liquid chromatography for the determination of anthraquinones in Radix et Rhizoma Rhei samples

In this article, a novel method termed as temperature-assisted ionic liquid dispersive liquid-liquid microextraction (TA IL-DLLME) combining high performance liquid chromatography with diode array detection (HPLC-DAD) was developed for the determination of anthraquinones in Radix et Rhizoma Rhei samples. The ionic liquid (1-hexyl-3-methylimidazolium hexafluorophosphate) was used to replace volatile organic solvent as an extraction solvent for the extraction of anthraquinones (aloe-emodin, rhein, emodin, chrysophanol and physcion) from Radix et Rhizoma Rhei. Several important parameters influencing the extraction efficiency of TA IL-DLLME such as the type and volume of extraction solvent and disperser solvent, sample pH, extraction time, extraction temperature, centrifugation time as well as salting-out effects were optimized. Under the optimal conditions, the spiked recovery for each analyte was in the range of 95.2-108.5%. The precisions of the proposed method were varied from 1.1% to 4.4% (RSD). All the analytes exhibited good linearity with correlation coefficients (r²) ranging from 0.9986 to 0.9996. The limits of detection for all target analytes were ranged from 0.50 to 2.02 μg L⁻¹ (S/N = 3). The experimental results indicated that the proposed method was successfully applied to the analysis of anthraquinones in Radix et Rhizoma Rhei.     

A new triterpene saponin from Panax japonicus C. A. Meyer var major (Burk.) C. Y. Wu et K. M. Feng

<正>One new triterpene saponin was isolated from Panaxjaponicus C.A.Meyer var major(Burk.) C.Y.Wu et K.M.Feng,and established as oleanolic acid 3-O-[β-D-glucopyranosyl-(1→2)-β-D-glucuronopyranosyl-6'-O-n-butyl ester]which showed moderate antitumor activities against the A2780 cells and OVCAR-3 cells.Its structure was established by means of spectral data, particularly NMR,including HSQC and HMBC techniques.     

不同品种砂仁挥发性成分及质量评价研究

采用气相色谱-质谱联用技术(GC-MS)对阳春砂、绿壳砂和缩砂的挥发性成分进行研究,分别鉴定出36、44、45种化学成分,并测定了其相对含量。采用色谱指纹图谱分区法,将砂仁总离子流色谱图分为3个区,对3个品种砂仁的质量进行分析和比较。结果表明,绿壳砂和缩砂的挥发性成分基本相同,而阳春砂与这两者的挥发性成分差异较大。阳春砂中含量最高的挥发性成分是砂仁的主要药效成分乙酸龙脑酯,其含量为59.60%。而绿壳砂和缩砂中含量最高的挥发性成分均为樟脑,分别占挥发性成分的63.02%和60.23%。阳春砂的品质最好,故不宜用绿壳砂或缩砂代替阳春砂入药。该研究为不同品种砂仁的鉴定及质量评价提供了新途径。     

HPLC测定河套大黄中的土大黄苷含量

从河套大黄中分离纯化出活性成分土大黄苷,作为自制的标准品,利用KromasilTM C(18)(250 mm×4.6 mm I.d.,5μm)反相色谱柱,以V(甲醇):V(乙腈):V(水)=35:5:60为流动相,以320mm为检测波长,对河套大黄中土大黄苷进行测定.土大黄苷在0.427～4.190μg范围内与峰面积呈良好线性关系(r=0.9994),平均回收率为99.12%.该方法为河套大黄的质量控制奠定了基础.     

大孔吸附树脂结合酶解法分离纯化虎杖中白藜芦醇的研究

研究了大孔吸附树脂结合酶解法提取和纯化虎杖中白藜芦醇的方法,采用HPLC法测定虎杖中白藜芦醇的含量,考查了β-糖苷酶对虎杖药材酶解前后白藜芦醇含量的变化,并经静态吸附考察了4种树脂,最后确定以H1020作为提取分离白藜芦醇的树脂.此树脂吸附量较高,脱附容易,有利于得到质量较好的白藜芦醇产品,经该树脂吸附解吸,饱和吸附量可达51.4mg/g,解吸率达92.5%.大孔树脂分离纯化白藜芦醇的含量可达71.5%,而上柱前粗提物中白藜芦醇含量为8.71%,说明采用本法分离纯化虎杖中白藜芦醇是可行的.     

Risk arbitrage in the Nikkei put warrant market of 1989–1990

This paper discusses the Nikkei put warrant market in Toronto and New York during 1989–1990. Three classes of long term American puts were traded which when evaluated in yen are ordinary, product and exchange asset puts, respectively. Type I do not involve exchange rates for yen investors. Type II, called quantos, fix in advance the exchange rate to be used on expiry in the home currency. Type III evaluate the strike and spot prices of the Nikkei Stock Average in the home currency rather than in yen. For typically observed parameters, type I are theoretically more valuable than type II which in turn are more valuable than type III. In late 1989 and early 1990 there were significant departures from fair values in various markets. This was a market with a set of complex financial instruments that even sophisticated investors needed time to learn about to price properly. Investors in Canada were willing to buy puts at far more than fair value based on historical volatility. In addition, US investors overpriced type II puts fixed in dollars rather than the type I's in yen. This led to cross border and US traded (on the same exchange) low risk hedges. The market's convergence to efficiency (that is, all puts priced within transaction cost bands) took about one month after the introduction of the US puts in early 1990 leading to significant profits for the hedgers.