光谱成像技术无损鉴别西洋参饮片的研究

应用电可控液晶光谱成像装置,测定不同市售来源的西洋参饮片,以期为其质量控制提供新的方法。系统光谱分辨率5nm,光谱覆盖范围为405～680nm,空间分辨率50lp·mm-1。从成像光谱立方体中提取特征光谱曲线,构建饮片指纹图谱;采用主成分等聚类分析方法解析其指纹图谱,用于饮片真伪鉴别与质量判定。结果与性状,显微及理化鉴定结果相吻合。表明光谱成像分析技术可用于中药指纹图谱的构建和质量评价,操作方法简便、快速、无损。     

Production, Characterization, and Application of an Organic Solvent-Tolerant Lipase Present in Active Inclusion Bodies

An organic solvent-tolerant lipase from Serratia marcescens ECU1010 (rSML) was overproduced in Escherichia coli in an insoluble form. High concentrations of both biomass (50 g cell wet weight/L culture broth) and inclusion bodies (10.5 g/L) were obtained by applying a high-cell-density cultivation procedure. Activity assays indicated that the enzymatic activity of rSML reached 600 U/L. After treatment with isopropyl ether for 12 h, the maximum lipase activity reached 6,000 U/L. Scanning electron microscopy and Fourier transform infrared microspectroscopy revealed the activation mechanism of rSML in the presence of organic solvents. rSML was stable in broad ranges of temperatures and pH values, as well as in a series of organic solvents. Besides, rSML showed the best enantioselectivity for the kinetic resolution of (±)-trans-3-(4-methoxyphenyl)glycidic acid methyl ester. These features render the S. marcescens ECU1010 lipase attractive for biotechnological applications in the field of organic synthesis and pharmaceutical industry.     

Effects of graft length and density of well‐defined graft polymers on the thermoresponsive behavior and self‐assembly morphology

A series of well‐defined thermoresponsive graft polymers with different lengths and graft densities, poly(glycidyl methacrylate)‐graft‐poly(N‐isopropylacrylate) (PGMA‐g‐PNIPAM), were successfully prepared by combination of controlled/living free radical polymerization and click chemistry. Effects of grafting length and density on the thermoresponsive behavior, aggregating mean diameter, and self‐assembly morphology are systematically investigated. The thermosensitive characteristics of graft polymers in aqueous solution prove that the length and graft density had positive co‐relationship with the lower critical solution temperature value and mean diameter of micelles as well as the size distribution, while the effect of graft length of polymers is more significant than that of density. Transmission electron microscopy analysis shows that the conformations of PGMA₄₅‐g‐PNIPAM₂₀ and PGMA₄₅‐g‐PNIPAM₄₆ with longer length and bigger grafting density in aqueous solutions are spherical nanoparticles with the increasing trend of the diameters, while that of PGMA₄₅‐g‐PNIPAM_{(73, 50%)} shows a spherical‐like morphology, which indicates that the graft length and density have a significant effect on the mean diameter of micelle but not on the self‐assembly morphology. These results reveal that to obtain desired thermoresponsive behavior and self‐assembly morphology of functional polymers, it is essential to design and fabricate the structure of graft polymers with proper length and graft density. © 2014 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2014 , 52, 2442–2453     

Quantification of complanatoside A in rat plasma using LC‐MS/MS and its application to a pharmacokinetic study

Complanatoside A is a flavonol glycoside isolated from Astragalus complanatus, and currently it is used as a quality control index for A. complanatus in the 2010 edition of the Chinese Pharmacopoeia. For the first time, a simple and sensitive LC‐MS/MS method was developed for the determination of complanatoside A in rat plasma over the range of 2.3–575 ng/mL. Complanatoside A was extracted from plasma by a protein precipitation procedure, separated by LC and detected by MS/MS in positive electrospray ionization mode. The method was validated for selectivity, carryover, sensitivity, linearity, extraction recovery, matrix effect, accuracy, precision and stability studies. The lower limit of quantification was established at 2.3 ng/mL. Intra‐ and inter‐day precisions (LLOQ, low‐QC, med‐QC and high‐QC) were <7.9%, and accuracies were between 94.0 and 105.1%. Matrix effect was acceptable (97.9–103.0%) and extraction recovery was reproducible (88.5–94.4%). Complanatoside A was stable in the investigated conditions. The method was applied to the pharmacokinetics of complanatoside A in rats. Copyright © 2015 John Wiley & Sons, Ltd.     

离子色谱法测定甲醇和噻吩中硫、氯含量

建立了测定工业用甲醇和噻吩中硫、氯含量的离子色谱检测方法。样品经(700±25)℃灼烧后,残留物用蒸馏水洗涤,利用离子色谱仪进行分析。甲醇和噻吩中硫、氯检测结果的相对标准偏差为1.04%~1.26%,加标回收率为99.2%~101.2%。该方法操作简单,精密度和准确度高,可用于大部分可燃性有机化合物中硫、氯含量的检测。     

Amperometric detection of nitrite based on Dawson-type vanodotungstophosphate and carbon nanotubes

A nitrite sensor based on Dawson vanodotungstophosphates α₂-K₇P₂VW₁₇O₆₂·18H₂O (P₂W₁₇V) and carbon nanotubes (CNTs) was prepared by electrostatic layer-by-layer self-assembly technique. The sensor {PEI/PSS/[PDDA/P₂W₁₇V-CNTs]_n} was characterized by UV–vis spectroscopy, atomic force microscopy (AFM), scanning electron microscopy (SEM) and X-ray photoelectron spectra (XPS). The electron transfer and sensing ability of this sensor were explored using cyclic voltammetry (CV) and electrochemical impedance spectra (EIS) technology. The results show that the incorporation of CNTs and P₂W₁₇V into the composite film endowed the modified electrode with fast transfer rate and high electrocatalytic activity towards oxidation of nitrite. This nitrite sensor with 10 bilayers has a broad linear range of 5 × 10⁻⁸ to 2.13 × 10⁻³ M, a low detection limit of 0.0367 μM (S N⁻¹ = 3), a high sensitivity of 0.35 mA mM⁻¹ NO₂⁻, an excellent anti-interference property in the presence of other potential interfering species and a good stable. It was successfully employed for determination of nitrite in real towards.     

Synthesis and comparative study of the heterocyclic rings on liquid crystalline properties of 2,5-aryl-1,3,4-oxa(thia)diazole derivatives containing furan and thiophene units

A series of heterocyclic liquid crystalline compounds containing 1,3,4-oxadiazole/thiadiazole, furan and thiophene units were synthesised and characterised by means of electrospray ionisation-mass spectrometry (ESI-MS), high-resolution mass spectroscopy (HRMS), ¹H nuclear magnetic resonance (NMR) and ¹³C NMR. The thermal behaviours were investigated by differential scanning calorimetry (DSC) and polarised optical microscopy (POM). The effect of the 1,3,4-oxadiazole, 1,3,4-thiadiazole, furan, thiophene and benzene rings on the liquid crystalline properties was discussed briefly in context with the geometrical and electronic factors. The results showed that the tendency to form mesophases follows the sequence: 1,4-disustituted benzene >2,5-disubstituted thiophene >2,5-disustituted furan and 1,3,4-thiadiazole >1,3,4-oxadiazole.     

Synthesis and liquid crystalline properties of substituted 2,5‐diaryl 1,3,4‐oxadiazole derivatives without flexible chains

A series of new compounds based on aromatically 2,5‐disubstituted 1,3,4‐oxadiazoles without flexible chains, formulated as p‐R–C₆H₄–(OC₂N₂)–(p‐C₆H₄)₂–R′ with (i) R = CH₃O, R′ = CH₃O, CH₃S, F, H (Ia–Id), (ii) R = CH₃S, R′ = CH₃O, CH₃S, F, H (IIa–IId) and (iii) R = F, R′ = CH₃O, CH₃S, F, H (IIIa–IIId) (p‐C₆H₄ and OC₂N₂ represent a p‐phenylene spacer and a 1,3,4‐oxadiazole ring, respectively), were synthesised and characterised by ¹H and ¹³C NMR, MS and HRMS techniques. Mesomorphic properties were investigated using differential scanning calorimetry and polarizing optical microscopy. All of the target compounds (except Id, IId, IIIc and IIId) exhibited an enantiotropic nematic mesophase with high melting temperatures. The liquid crystalline properties of these compounds were influenced greatly by polarity, steric factors and positions of the terminal groups. The effect of the terminal groups on the liquid crystal properties is discussed.