高分离度快速液相色谱法测定牛黄解毒片中黄芩苷的含量

采用高分离度快速液相色谱(RRLC)测定牛黄解毒片中黄芩苷的含量。色谱柱为Zorbax XDB-C18(4.6×50mm,1.8μm),流动相为甲醇-水-磷酸(45∶55∶0.2),检测波长315nm,流速0.5mL.min-1,柱温为30℃。黄芩苷在0.15—1.35μg(r=0.9999)范围内峰面积与浓度呈良好的线性关系,加样回收率为100.41%,RSD=1.42%。采用高分离度快速液相色谱(RRLC)测定复方牛黄解毒片中黄芩苷的含量,缩短了保留时间,提高了效率,降低了成本。本方法简便、准确,结果稳定。     

Aromatic nitro substitution reaction between 4‐nitro‐N‐n‐butyl‐1,8‐naphthalimide and n‐heptanethiol in water–methanol binary mixtures

The second‐order rate constants of thiolysis by n‐heptanethiol on 4‐nitro‐N‐n‐butyl‐1,8‐naphthalimide (4NBN) are strongly affected by the water–methanol binary mixture composition reaching its maximum at around 50% mole fraction. In parallel solvent effects on 4NBN absorption molar extinction coefficient also shows a maximum at this composition region. From the spectroscopic study of reactant and product and the known H‐bond capacity of the mixture a rationalization that involves specific solvent H‐donor interaction with the nitro group is proposed to explain the kinetic data. Present findings also show a convenient methodology to obtain strongly fluorescent imides, valuable for peptide and analogs labeling as well as for thio‐naphthalimide derivatives preparations. Copyright © 2008 John Wiley & Sons, Ltd.     

Insights into the Antimicrobial Activity of Hydrated Cobaltmolybdate Doped with Copper

Molybdates are biocidal materials that can be useful in coating surfaces that are susceptible to contamination and the spread of microorganisms. The aim of this work was to investigate the effects of copper doping of hydrated cobalt molybdate, synthesized by the co-precipitation method, on its antibacterial activity and to elucidate the structural and morphological changes caused by the dopant in the material. The synthesized materials were characterized by PXRD, Fourier Transformed Infrared (FTIR), thermogravimetric analysis/differential scanning calorimetry (TG/DSC), and SEM-Energy Dispersive Spectroscopy (SEM-EDS). The antibacterial response of the materials was verified using the Minimum Inhibitory Concentration (MIC) employing the broth microdilution method. The size of the CoMoO₄·1.03H₂O microparticles gradually increased as the percentage of copper increased, decreasing the energy that is needed to promote the transition from the hydrated to the beta phase and changing the color of material. CoMoO₄·1.03H₂O obtained better bactericidal performance against the tested strains of Staphylococcus aureus (gram-positive) than Escherichia coli (gram-negative). However, an interesting point was that the use of copper as a doping agent for hydrated cobalt molybdate caused an increase of MIC value in the presence of E. coli and S. aureus strains. The study demonstrates the need for caution in the use of copper as a doping material in biocidal matrices, such as cobalt molybdate.     

Synthesis and characterization of CeO<Subscript>2</Subscript>–graphene composite

The synthesis and characterization of graphite oxide (GO), graphene (GS), and the composites: GS–CeO₂ and GO–CeO₂ are reported. This synthesis was carried out by mixing aqueous solutions of CeCl₃·7H₂O and GO, which yields the oxidized composite GO–CeO₂. GO–CeO₂ was hydrothermally reduced with ethylene glycol, at 120 °C, yielding the reduced composite GS–CeO₂. GO, GS ,and the composites with CeO₂ were characterized by CHN, TG/DTG, BET, XRD, SEM microscopy, FTIR, and Raman spectroscopy. The estimation of crystallite size of CeO₂ anchored on GO and on GS by Raman, XRD, and SEM agreed very well showing diameters about 5 nm. The role of particles of CeO₂ coating carbon sheets of GO and GS was discussed.     

Tryptophan photooxidation promoted by new hybrid materials prepared by condensation of naphthalene imides with silicate by the sol–gel process

Three novel hybrid organic/inorganic materials were synthesized from 4-substituted (NO₂, Br, H) 1,8-naphthalene imide-N-propyltriethoxysilane by the sol–gel process. These materials were obtained as a xerogel and partially characterized. The ability to photosensitize the oxidation and degradation of tryptophan indole ring by these materials was studied through photophysical and photochemical techniques. Although the derivatives containing Br and NO₂ as substituent do not cause efficient tryptophan photodamage, the hybrid material obtained from 1,8-naphthalic anhydride is very efficient to promote tryptophan photooxidation. By using laser flash photolysis it was possible to verify the presence of naphthalene imide transient radical species. The presence of oxygen causes an increase of the yield of radical formation. These results suggest that the mechanism of photodegradation of tryptophan occurs by type I, i.e. the transient radical (TrpH⁺) formed by the direct reaction of the triplet state of the naphthalene imide moiety with tryptophan. Thus a inorganic–organic hybrid material that can be used to promote the oxidation of biomolecules was obtained.     

Detection of bacteria using antimicrobial polymer derived via ring-opening metathesis (romp) pathway

There is growing interest in the detection of bacteria in consumables, for example, in the food and water sectors. In this study, the aim was to produce a polymer-based bacteria biosensor via ROMP (ring opening metathesis polymerization). In the first part of the study, block and random copolymers were synthesized, and their biocidal activities were tested on the glass surface. Interdigitated electrode arrays coated with the polymers possessing the highest activity were used to screen the affinity towards different bacterial strains by monitoring impedance variations in real-time. The polymer-coated electrode could detect gram-positive and gram-negative bacteria strains at a concentration of 10⁷ cfu/mL. The results show that ROMP-based polymer offers bacterial detection and can be used in developing biosensor devices for efficiently detecting pathogenic bacteria.     

Supercritical carbon dioxide extraction of Usnea longissima (L.) Ach.: Optimization by Box-Behnken design (BBD)

Usnic acid (UA) was extracted from Usnea longissima (L.) Ach. in supercritical carbon dioxide (SC-CO₂) medium. The selected process parameters were extraction temperature (35–45 °C), amount of co-solvent (0%–5%) and extraction time (5–9 h). These parameters were applied to Box-Behnken design (BBD) belonging to response surface methodology (RSM) to determine optimum process parameters for the highest amount of UA in the extract. g UA/100g lichen, extraction yield % and UA content values were calculated in the range of 0.045–0.317, 2.77–5.4 and 71%–82% in different experimental conditions, respectively. The optimum conditions were predicted as 42 °C, 4.3% (ethanol) and 7.48 h. It was determined that the predicted and experimental values of g UA/100g lichen were compatible, and the suggested model was valid.