Carboxylated graphene oxide/polyvinyl chloride as solid-phase extraction sorbent combined with ion chromatography for the determination of sulfonamides in cosmetics

A carboxylated graphene oxide/polyvinyl chloride (CGO/PVC) material was prepared as a sorbent for the selective extraction of sulphonamides from complex sample. After being dispersed in buffer solution, sample was transferred into the prefabricated solid-phase extraction (SPE) column, which integrated extraction and cleanup into one single-step. A multi-response optimization based on the Box-Behnken design was used to optimize factors affecting extraction efficiency. Compared with the commonly commercial sorbents including MCX, WCX and C₁₈, CGO/PVC hybrid material had higher extraction selectivity and capacity to sulphonamides. The limits of detection and quantification for seven target compounds were in the range of 3.4–7.1 μg/L and 11.4–23.7 μg/L, respectively. The self-assembly SPE cartridge was successfully used to enrich seven analytes in anti-acne cosmetics prior to ion chromatography detection with good recoveries of 87.8–102.0% and relative standard deviations of 1.2–6.4%, implying that this method was suitable for routine analysis of cosmetics.     

Isolation and Characterization of Secondary Metabolites from Rhododendron microphyton

Four new iridoids, incarvoids D–F ( 1 – 3 , resp.) and incarvoid B 9‐O‐β‐D ‐glucopyranoside ( 4 ), and one new monoterpenoid, argutoid B ( 5 ), along with 14 known compounds, were isolated from Rhododendron microphyton. Their structures were established by comprehensive 1D‐ and 2D‐NMR spectroscopic analysis.     

固体核磁共振研究分子筛的新进展

分子筛由于具有独特的孔道及可调控酸碱性等特征,被作为离子交换剂、吸附剂及催化剂而广泛应用于石油化工的各种催化过程中。固体核磁共振是研究分子筛结构、酸性及主客体相互作用的强有力谱学手段之一。简单概述了固体核磁共振研究分子筛的最近进展。     

Flame-retardant Wrapped Ramie Fibers towards Suppressing “Candlewick Effect” of Polypropylene/Ramie Fiber Composites

In this work, a flame-retardant polypropylene(PP)/ramie fiber(RF) composite was prepared. The ramie fibers were wrapped chemically by a phosphorus- and nitrogen-containing flame retardant(FR) produced via in situ condensation reaction so as to suppress their candlewick effect. Fourier transform infrared spectroscopy(FTIR), X-ray photoelectron spectroscopy(XPS) and scanning electron microscopy(SEM) demonstrated that the ramie fibers wrapped chemically by FR(FR-RF) were obtained successfully. Thermogravimatric test showed that the PP/FR-RF composite had more residue and better thermal stability at high temperatures than the PP/RF composite. Cone calorimeter(CC) results indicated that the peak of heat release rate(PHRR) and total heat release(THR) correspondingly decreased by 23.4% and 12.5% compared with the values of neat PP/RF. The PP/FR-RF composite created a continuous and compact char layer after the combustion. Combining FTIR analysis of char residue after CC test with heat conduction coefficient results, it could be concluded that the charring of FR on RF greatly weakened the candlewick effect of RF, and more char residue in the RF domain facilitated the formation of more continuous and compact char layer in the whole combustion zone, consequently protected PP composites during combustion, resulting in the better flame retardancy of PP/FR-RF composite than that of PP/RF composite.     

Flow-injection chemiluminescence method for determination of critical micelle concentration of surfactants

In this study, chemiluminescence (CL) behaviour of Luminol-H₂O₂ in the presence of the different concentrations of four surfactants, cetyltrimethylammonium bromide (CTAB), cetylpyridinium bromide (CPB), sodium dodecyl sulphate (SDS) and polyoxyethylene dodecyl ether (Brij-35), was investigated. A novel method for the direct determination of critical micelle concentration (CMC) of the surfactants using flow-injection CL is described. Under the optimum conditions, the luminescence intensity of the Luminol-H₂O₂ system increased gradually with increasing concentration of the surfactants before the CMC, but rapidly reached to the emission maximum at the CMC, followed by a decrease after the CMC. The concentrations of the surfactants corresponding to the luminescence maximum are in agreement with the literature CMC values. The main factors affecting the determination of CMC are discussed. The mechanistic studies show that the luminescence peaks observed in the experiment were mainly because of the protective effect of the micelle against the transition of the excited species and the retarding effect of the micelle structures on the CL reaction rate.     

Density of lithium fluoride—lithium carbonate-based molten salts

The density of the LiF-Li₂CO₃ melts system was measured using the Archimedean method. Using the quadratic regression orthogonal design with two factors, a regression equation for the density of LiF-Li₂CO₃ melts was obtained in which the concentration of LiF and temperature were considered. The results indicated that the density of the LiF-Li₂CO₃ melts decreased with either increasing the concentration of LiF or increasing temperature; a linear relation was observed between density and temperature. In addition, the influences of NaF, KF, NaCl, and KCl additives on the densities of the given systems were studied. The addition of NaF and KF increased the density of the melts, whereas NaCl and KCl resulted in an initial increase and subsequent decrease with an increasing additive concentration. The density attained a maximum at NaCl and KCl mass fraction of approximately 15%.     

Reaction kinetics of malachite in ammonium carbamate solution

The dissolution of malachite particles in ammonium carbamate (AC) solutions was investigated in a batch reactor, using the parameters of temperature, AC concentration, particle size, and stirring speed. The shrinking core model was evaluated for the dissolution rate increased by decreasing particle size and increasing the temperature and AC concentration. No important effect was observed for variations in stirring speed. Dissolution curves were evaluated in order to test shrinking core models for fluid-solid systems. The dissolution rate was determined as being controlled by surface chemical reaction. The activation energy of the leaching process was determined as 46.04 kJ mol^?1.     

铜催化α-重氮酮对硼氢键的不对称插入反应

手性有机硼化合物在有机合成、医药、材料等诸多领域中有广泛的应用,发展该类化合物的高效合成方法一直广受关注.此前,我们发展了过渡金属催化卡宾对硼氢键(B—H)的插入反应,并实现了α-重氮酯对B—H键的不对称插入反应.本文以手性螺环双噁唑啉配体和铜的络合物作为催化剂,首次实现了α-重氮酮对膦-硼烷加合物的B—H键不对称插入反应,获得了较高的收率和高达83%ee的对映选择性.该研究成果是为数不多的以α-重氮酮作为卡宾前体的不对称杂原子氢键插入反应,为手性α-硼取代酮化合物这类新的有机硼化合物的合成提供了有效方法.     

Total Syntheses of (−)‐Isoschizogamine and (−)‐2‐Hydroxyisoschizogamine

Total syntheses of (?)‐isoschizogamine and (?)‐2‐hydroxyisoschizogamine are described. The synthesis employs two asymmetric Michael additions to establish chiral centers at C7 and the quaternary carbon C20. Regioselective reduction of the methylthioiminium cation rather than the enamine generates an isoschizogamine‐type pentacyclic skeleton. Acidic hydrolysis of the isoschizogamine‐type intermediate in the absence of oxygen provides natural (?)‐isoschizogamine. Conducting the reaction in the presence of oxygen leads to a multistep oxidative hydrolysis cascade that affords unnatural (?)‐2‐hydroxyisoschizogamine.