Regio- and Stereocontrolled Nucleophilic Addition Reactions of An Unsymmetrically Disbustituted Butadiene η4-Molybdenum Cationic Complex

The reactions of a new cationic complex, [Cp(CO)₂Mo(η⁴-2-methyl-3-SPh-C₄H₄)]⁺ PF^?₆ (3), with carbon, hydride, and nitrogen nucleophiles were found to give only the C-1 addition products in good yield. The X-ray crystal structures of two of the addition products 4a and 4e confirm the regio- and stereochemistry of the nucleophilic additions.     

Novel Rearrangements of 2,3-Dimercapto-1-propanol Derivatives: Formation of Dialkyl Sulfide, Dialkyl Disulfide, and 1,2,3-Tris(alkylthio)propane

The base alkylation of 2,3-dimercapto-1-propanol with alkyl halides leads in good yield to 2,3-bis(alkylthio)-1-propanol and dialkyl sulfide. The reaction of 2,3-bis(alkylthio)-1-propanol with catalytic concentrated sulfuric acid proceeds with rearrangement to give 1,2,3-tris(alkylthio)propane and dialkyl disulfide. The rearrangement reaction takes place through a common intermediate thiaranium intermediate 8.     

A validated HPLC method with ultraviolet detection for the determination of buformin in plasma

A sensitive and rapid high-performance liquid chromatographic assay is developed and validated for the determination of buformin in plasma. After addition of metformin as the internal standard, the analytes were deproteinated with acetonitrile, washed with dichloromethane, and the resulting supernatant injected. Chromatography was performed at ambient temperature by pumping a mobile phase of 0.03 m diammonium hydrogen phosphate buffer (pH 7, 250 mL) in methanol (750 mL) at a fl ow rate of 1 mL/min through a silica column. Buformin and metformin were detected at 236 nm, and eluted 9.8 and 15.4 min, respectively. No endogenous substances were found to interfere. Calibration curves were linear over the concentration range of 20-2000 ng/mL. The limit of quantitation was 20 ng/mL. The intra- and inter-day relative standard deviation (RSD) was 8.3%, or less, and the accuracy was within 10.1% of the relative error (RE). The method is suitable in pharmacokinetic investigation of buformin.     

Effect of take-up speed on physical properties and permeation performance of cellulose acetate hollow fibers

Cellulose acetate (CA) ultrafiltration hollow fibers were spun via the dry-jet wet spinning technique. The effect of the take-up speed on the mechanical properties, morphology, thermal properties, pure water permeation, retention, and surface characterization of hollow fiber membranes were investigated. Both the inner and outer diameters of the hollow fiber decreased with the increase of take-up speed. Macrovoids were observed on the inner surface of the drawn hollow fibers. The d-space decreased with the increase of the take-up speed. The ultimate tensile stress (UTS) increased and the breaking elongation decreased with the increase of take-up speed. The permeation performance was measured. The hydraulic permeability increased and the retention decreased slightly with the increase of the take-up speed. The surface roughness increased with the increase of the take-up speed. The thermal analysis results showed that the endothermic peak shifts to the higher temperature region and coefficient of thermal expansion (CTE) decrease for a higher take-up speed.     

Speciation of bound and free metals evaluated for lobster digestive gland extracts

A simple method is described for the speciation of metalions in biological extracts with a short desalting gel-filtration column. The system was optimized for the eluent and gel type to provide accurate free metal ion levels and minimum processing times. The four separation media studied were Sephadex G25, Bio-Gel P-6DG, controlled pore glass CPG40, and Fractogel HW40F. The best medium was the Fractogel HW40F because it was not compressible and allowed a pump to be used to obtain uniform flow rates. The eluent was 0.10 M ammonium acetate/0.01 M citric acid adjusted to pH 7.0. This eluent minimized ion/gel interactions and gave a lower salt content relative to other possible eluents. The separation time was 10 min per sample per metal ion of interest. The detection limits relative to the mass of wet tissue for the column/flame spectrometer system were 0.80 μg g^?1, 0.80 μg g^?1, and 1.6 μg g^?1 for zinc, cadmium and copper, respectively. The method is evaluated for a lobster digestive gland extract; the methodology should be applicable to other systems containing nonlabile metal species.     

Effects of Different Extraction Methods on Vanilla Aroma

To establish the analytic conditions for examining the aroma quality of vanilla pods, we compared different extraction methods and identified a suitable option. We utilized headspace solid-phase microextraction (HS-SPME), steam distillation (SD), simultaneous steam distillation (SDE) and alcoholic extraction combined with gas chromatography (GC) and gas chromatography–mass spectrometry (GC-MS) to identify volatile components of vanilla pods. A total of 84 volatile compounds were identified in this experiment, of which SDE could identify the most volatile compounds, with a total of 51 species, followed by HS-SPME, with a total of 28 species. Ten volatile compounds were identified by extraction with a minimum of 35% alcohol. HS-SPME extraction provided the highest total aroma peak areas, and the peak areas of aldehydes, furans, alcohols, monoterpenes and phenols compounds were several times higher than those of the other extraction methods. The results showed that the two technologies, SDE and HS-SPME, could be used together to facilitate analysis of vanilla pod aroma.