Volatiles from Thymbra and Thymus species of the western Mediterranean basin, Portugal and Macaronesia

Thyme is the common name of many taxa belonging to the Thymbra and Thymus genera. Given the economic importance of thyme oils, many thyme species have been studied and their essential oils and other volatile-containing extracts chemically characterized. Thymbra and Thymus species are frequent in the west Mediterranean region, considered to be the centre of origin of the genus Thymus, and extend further westwards in the Iberian Peninsula and northwest Africa, to the Macaronesian region in the Atlantic Ocean. The present work gives an overview of the chemical composition of the volatiles from the taxa of these two genera occurring in the above geographic area.     

Analysis of phenylpiperazine-like stimulants in human hair as trimethylsilyl derivatives by gas chromatography–mass spectrometry

A simple and sensitive procedure, using p-tolylpiperazine (pTP) as internal standard (IS), has been developed and validated for the qualitative and quantitative analysis of 1-(3-trifuoromethylphenyl)piperazine (TFMPP), 1-(3-chlorophenyl)piperazine (mCPP) and 1-(4-methoxyphenyl)piperazine (MeOPP) in hair. Drug extraction was performed by incubation with 1 M sodium hydroxide at 50 °C for 40 min, and the extracts were cleaned up using mixed-mode solid-phase extraction. The analytes were derivatized with N-methyl-N-(trimethylsilyl) trifluoroacetamide with 5% trimethylchlorosilane and analysed by gas chromatography–mass spectrometry in the selected ion monitoring mode. The method was linear from 0.05 (lower limit of quantitation) to 4 ng mg⁻¹, with correlation coefficients higher than 0.99 for all the compounds. Intra- and interday precision and accuracy were in conformity with the criteria normally accepted in bioanalytical method validation, and the sample cleanup step presented a mean efficiency higher than 90% for all the analytes. Due to its simplicity and speed, this method can be successfully applied in the screening and quantitation of these compounds in hair samples, and is suitable for application in forensic toxicology routine analysis.     

无零级衍射干扰的彩色数字全息研究

彩色数字全息研究中,用球面波为重建波及角谱衍射公式进行波前重建是一种有效的方法.然而,重建图像上通常伴有强烈的零级衍射干扰.本文通过理论分析,对波前重建过程作了重要改进.用改进后的方法进行彩色数字全息的实验研究表明,重建彩色图像的质量获得显著改善. 关键词： 彩色数字全息 波前重建 零级衍射干扰     

Synthesis of partially benzylated arabinofuranosides,NMR analysis,and application to oligosaccharide synthesis

The preparation and NMR analysis of 2,3-di-O-benzyl arabinofuranosides have been described. In DMSO-d₆, the sugar adopts a conformation in which the hydroxyl groups are in an equatorial position; the equilibrium composition is determined by steric factors. In CDCl₃, the sugar adopts a conformation in which the intramolecular hydrogen bonding plays an important role in determining the equilibrium composition. The use of 2,3-di-O-benzyl arabinose in the synthesis of oligoarabinofuranosides enabled the synthesis of α- or β-linked furanosides.     

Iron-catalyzed selective reduction of nitro compounds to amines

An efficient reduction of the nitro group with a catalytic amount of Fe(acac)₃ and TMDS in THF at 60 °C affording the corresponding amine is described.     

Concentration multi-échelles de courbure dans des fibres de Milnor

Résumé. Etant donné un germe de morphisme analytique complexe à fibre réduite, nous étudions la manière dont la courbure de Lipschitz-Killing de la fibre de Milnor pour la métrique induite par celle de se concentre asymptotiquement, lorsque , dans l'intersection de cette fibre avec des boules dont les centres peuvent être décrits mais surtout dont les rayons sont de la forme où les des nombres rationnels dont la collection ne dépend que de la topologie du plongement dans du germe de courbe plane réduite . Received: May 29, 1998.     

Ultrasound-assisted extraction and determination of tartaric and malic acids from grapes and winemaking by-products

The optimization of an ultrasound-assisted extraction (UAE) method for tartaric and malic acids from grape derived samples is shown. A fractional factorial experimental design allowed for the determination of the effects of seven extraction variables. Relationships between all the variables were examined. By applying graphical analysis, the best extractions conditions were obtained. The most important variables were the extracting liquid and the extraction temperature. Later, a central composite design was applied for optimizing the temperature and the composition of the extracting liquid. The optimized method was applied to grapes and to winemaking by-products. The repeatability of the method was studied and the recovery of tartaric and malic acids was established. Organic acids quantification was done by liquid chromatography (LC) using a post-column buffer and a conductivity detector.     

The preopt package for pre-optimization of gradient elutions in high-performance liquid chromatography

A theoretical model is described for quick pre-optimization of binary multistep gradient elutions in liquid chromatography. This model utilizes experimental retention-time data under isocratic elution conditions for different proportions of organic modifier in the mobile phase, and simulates the position of the peaks in the chromatogram by calculation of the average velocity of the peaks through the column. Optimization is done for multistep gradients by means of the simplex algorithm. The results must then be confirmed experimentally. Results are given demonstrating the power and validity of the model in the resolution of complex mixtures. The whole process done on a micro-computer with the PREOPT package usually takes about 30 min, without requiring user participation or chromatographic instrumentation.     

On the Synthesis of Pyrrolobenzo[<Emphasis Type="Italic">b</Emphasis>]thieno[1,4]diazepines

Summary. 2-Amino-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carbonitrile was converted into the corresponding 2-(pyrrol-1-yl) derivative, followed by reduction of the latter compound into the corresponding amine. This amine and its acyl, aroyl, and arylidene derivatives were used as synthons in the synthesis of several title compounds.