In-tube solid-phase microextraction with poly(methacrylic acid-ethylene glycol dimethacrylate) monolithic capillary for direct high-performance liquid chromatographic determination of ketamine in urine samples

Ketamine was used for anaesthesia originally but has emerged as an abused drug in recent years. The prevalence of ketamine abuse demands a direct and rapid determination method. It is known that in-tube solid phase microextraction (in-tube SPME) can perform extraction with a capillary linked directly to a HPLC system, providing an automated and accurate extraction procedure. In this paper, an in-tube SPME coupled to HPLC method was developed for the determination of ketamine in urine samples with a poly(methacrylic acid-ethylene glycol dimethacrylate) monolithic capillary column as the extraction phase, which is expected to provide higher extraction efficiency than open tubular capillaries. After optimizing the extraction conditions, ketamine was extracted directly from urine samples in a wide dynamic linear range of 50-10,000 ng mL(-1), with the detection limit obtained as 6.4 ng mL(-1). The intra-day and inter-day precision for the method was 1.6% and 1.7%, respectively. The urine samples from suspect addicts have been successfully analyzed within 20 min. The re-usability of the monolithic column was also confirmed as no decrease of the extraction efficiency was shown after urine extraction.     

Ion-driven ATP pump by self-organized hybrid membrane materials

We report new hybrid organic-inorganic materials, based on macrocyclic receptors 1-3 self-organized in tubular superstructures prepared by sol-gel process. Fourier transform infrared (FTIR) and NMR spectroscopic analyses demonstrate that the self-organization by hydrogen bonding of organogel superstructures of 2 and 3 were preserved in the hybrid materials throughout the sol-gel process. The molecular arrangement of heteroditopic receptors defines a particularly attractive functional transport device for both cation (tubular macrocycles) and anion (sandwich-urea) directional-diffusion transport mechanism in the hybrid membrane material. This system has been employed successfully to design a solid dense membrane, functioning as an ion-powered adenosine triphosphate (ATP(2)(-)) pump, and illustrates how a self-organized hybrid material performs interesting and potentially useful functions.     

核苷与碱基的苯胺甲基键合硅胶固定相高效液相色谱分离

建立苯胺甲基键合硅胶固定相(PAMS)高效液相色谱分离核苷与碱基的方法；研究流动相有机溶剂浓度、磷酸缓冲液pH值、离子强度对核苷和碱基在该键合固定相上的色谱保留及分离选择性的影响，用磷酸缓冲液(pH＝4)为流动相快速分离了部分核苷与碱基。     

Synthesis of novel halo-oxybispyridines, new building blocks in cholinergic medicinal chemistry

This paper describes a method for the preparation of oxybispyridines bearing several halogens, which could be further transformed into other functional groups thus giving access to libraries with the bis-pyridyl ether moiety as the common structural feature of interest in cholinergic medicinal chemistry. Scope and limitation of the method are outlined.     

Production of sulfur from gypsum as an industrial byproduct

Biological sulfate reduction was investigated at the bench and pilot scales in order to determine optimum culture conditions. Efficient strains of sulfate-reducing bacteria (SRB) were selected by classical microbiological methods and by mutagenesis. Improvement factors, including stripping, scale-up, sulfate, and organic substrate concentrations, have been studied in batch bioreactors.

Two types of pilot-scale bioreactors have been adopted, the first being completely mixed with free cells and the second having two stages with immobilized cells on a fixed bed. An overall bioconversion capacity of 11 kg/m³·d of gypsum and 1.2 kg/m³·d of dissolved organic carbon has been achieved in the two-stage bioreactor.

     

Two New Triterpene Esters from Daphniphyllum oldhami

Two new triterpene esters,2-O-eaffeoylalphitolic acid(1)and methyl 2-O-eaffeoyl-alphitolate(2),together with two known triterpenes were isolated from the shrub Daphniphyllum oldnami.The structures of new compounds were elucidated on the basis of detailed spectroscopic analysis and compared with related compound.     

Quantification of the 35S promoter in DNA extracts from genetically modified organisms using real-time polymerase chain reaction and specificity assessment on various genetically modified organisms, part I: operating procedure

A highly sensitive quantitative real-time assay targeted on the 35S promoter of a commercial genetically modified organism (GMO) was characterized (sF/sR primers) and developed for an ABI Prism 7700 Sequence Detection System and TaqMan chemistry. The specificity assessment and performance criteria of sF/sR assay were compared to other P35S-targeted published assays. sF/sR primers amplified a 79 base pair DNA sequence located in a part of P35S that is highly conserved among many caulimovirus strains, i.e., this consensus part of CaMV P35S is likely to be present in many GM events. According to the experimental conditions, the absolute limit of detection for Bt176 corn was estimated between 0.2 and 2 copies of equivalent genome (CEG). The limit of quantification was reached below 0.1% Bt176 content. A Cauliflower Mosaic Virus control (CaMV) qualitative assay targeted on the ORF III of the viral genome was also used as a control (primers 3F/3R) to assess the presence of CaMV in plant-derived products. The specificity of this test was assessed on various CaMV strains, including the Figwort Mosaic Virus (FMV) and solanaceous CaMV strains. Considering the performance of sF/sR quantification test, the highly conserved sequence, and the small size of the amplicon, this assay was tested in a collaborative study in order to be proposed as an international standard.     

A New Cyclic Bisdesmoside from Tubers of Bolbostemma paniculatum

The structure of tubeimoside V (1), a new cyclic bisdesmoside, isolated from tubers of Bolbostemma paniculatum (Tu Bei Mu), was established by means of 2D NMR spectral and chemical methods. Compound 1 has inter-saccharide chain bridging by a dicrotalic acid to form aunique macrocyclic structure.