不同微波膨胀烟梗的化学感官特性研究

研究不同来源包括产地、部位、年份、品种的烟梗原料经相同的微波膨胀工艺处理后的常规化学成分、致香成分、主流烟气(主要包括抽吸口数、焦油、烟碱及一氧化碳释放量)及感官特性差异,指导微波膨胀梗丝在产品中的配伍应用,为建立不同来源微波膨胀梗原料的品质特征评价体系及微波膨胀梗丝的工业应用提供依据。结果表明:不同产地来源的微波膨胀梗丝常规化学成分、致香成分、主流烟气存在差异。不同年份的微波膨胀梗丝间感官质量无明显差异,不同产地、品种、部位来源的微波膨胀梗丝总体感官质量存在差异。     

Routine Analysis of Catecholamines and Metabolites in Urine by a Liquid Chromatographic Column Switching System

Abstract

A reversed-phase liquid chromatographic technique including a column switching system has been adapted for the routine measurement of catecholamines and their metabolites (14 compounds) in urine. From 1 ml of urine all the compounds and the internal standards were obtained according to combined extraction procedures involving organic solvent, anionic and weakly cationic resins. Finally four extracts (catecholamines, methoxamines, acidic and neutral derivatives) had to be chromatographed throughout a wholly automated apparatus. For each run, the column switching system determined the analytical columns to be used to obtain the separation of the compounds from interferences due to other co-extracted endogenous substances, while the analysis times remained between 20 and 40 min. Such a system allowed the rapid clean-up of columns (in direct- and back-flush mode) carried out between two consecutive injections. By coupling on-line fluorimetric and electro-chemical detections the specificity of the technique could be checked, since the ratio of the responses of both detectors was an index of the purity of the peaks. Finally the advanced automation of the equipment allowed weekly the evaluation of catecholamines and the whole range of their known metabolites in 36 urine samples.     

用于考察外源添加剂对卷烟常规烟气指标影响的样品制备因子筛选

为筛选用于考察外源添加剂对卷烟常规烟气指标影响的样品制备关键控制因子,采用L_8(2~7)正交试验设计进行香兰素及乙基麦芽酚的添加实验.卷烟常规烟气指标变化数值通过极差分析、方差分析,结果显示:参比卷烟种类是影响卷烟烟气总粒相物、焦油、水分的高度显著因子,就试验采用的1R5F和3R4F参比卷烟而言,添加剂在高焦油3R4F卷烟中对常规烟气指标的影响比其在低焦油1R5F卷烟中的影响大;添加剂种类与浓度的交互作用不仅对卷烟烟气总粒相物有高度显著影响,而且对总粒相物中的水分也有显著影响;因此,规范样品制备,可减少误差、保证后续外源添加剂加入对卷烟常规烟气指标影响评价结果和推断的可靠性及科学性.     

Optimization of sampling frequency for routine river water quality monitoring

Sampling frequency is an important factor to be considered during the design of a water monitoring network,and the cost-effective selection of possible ways and means for the optimization of sampling frequency is still needed.This paper introduces water pollution index deviation ratio comparison(WPI DRC),a procedure for the optimization of sampling frequency for a routine river water quality monitoring system.Sampling frequency optimized using WPI DRC at monitoring station X5 in the mainstream of Xiangjiang River is compared with that established using the traditional Statistical Algorithm method.The result of comparison indicates that WPI DRC is more feasible than the traditional one.And then,the sampling frequencies for other 16 monitoring stations also have been optimized,and the results show the sampling frequencies of all the stations except that X4 are reduced,and there is no unacceptable difference between water quality evaluation results at 17 stations before and after the optimization.Therefore,it is concluded that WPI DRC is an effective optimization process with operable results,which can be used to fulfill the requirement of practical monitoring work.     

基于串联反应的吡虫啉新合成工艺研究

以2-氯-5-氯甲基吡啶(CCMP)、无水乙二胺和硝基胍为原料,运用串联反应方法合成了吡虫啉[化学名:1-(6-氯-3-吡啶甲基)-N-硝基-2-咪唑啉亚胺]。该方法反应中间体无需纯化处理,操作简单,同时解决了活性中间体进一步进行副反应的难题。通过单因素实验,探讨了pH、反应溶剂、温度以及时间等因素对产物收率的影响,得到的优化工艺条件为:以乙腈为溶剂,nCCMP∶n无水乙二胺∶n硝基胍=1∶5∶1,于30℃反应120min,产率可达96.35%。其结构经1H NMR、13C NMR、IR表征。     

New practical tools for the implementation and use of ultrafast 2D NMR experiments

Ultrafast (UF) 2D NMR is a very promising methodology enabling the acquisition of 2D spectra in a single scan. In the last few years, the analytical performance of UF 2D NMR has been highly increased, consequently maximizing its range of applications. However, its implementation and use by non‐specialists are far from being straightforward, because of the specific acquisition and processing procedures and parameters characterizing UF NMR. To make this methodology implementable and applicable by non‐specialists, we developed a simple routine capable of translating conventional parameters (spectral widths and transmitter frequencies) into specific UF parameters (gradient and chirp pulse parameters). This macro was subsequently implemented in a Web page, which is available for external users. Although the algorithm was designed for two widely used 2D experiments, COSY and HSQC, it can easily be extended to any other pulse sequence. The robustness of this routine was verified successfully on a variety of small molecules. We believe that this tool will eliminate much of the technical difficulties related to UF 2D NMR and will make the technique accessible to a wider audience of organic and analytical chemists. Copyright © 2013 John Wiley & Sons, Ltd.     

[Ni（H2O）（tptz）（C2O4）]·4H2O的合成、结构与表征

在CH3OH／H2O混合溶剂中，经2，4，6-三（2-吡啶基）-1，3，5-三嗪（tptz）、草酸和新制Ni（OH）2／NiCO3反应合成得到配合物[Ni（H2O）（tptz）（C2O4）]·4H2O．单晶X-射线衍射分析表明：它与已报道的[M（H2O）（tptz）（C2O4）]·4H2O（M=Co（2）、Cu（3）、Zn（4））配合物同晶形，属三斜晶系，P1空间群，晶胞参数a=7．760（2）A，b=12．116（2）A，c=13．031（3）A，α=78．76（4）°，β=83．84（3）°，γ=78．69（3）°，V=1175．3（5）A^3，Z=2，Dc=1．543，F（000）=562，R1=0．0472，wR2=0．1350，GOF=1．088．在配合物的结构基础上与同晶形结构进行比较分析，并研究了它们的IR及TG／DTA测试表征．     

惯例复制与知识转移:作用机制的权变条件研究

针对惯例复制过程中与外部情景难以匹配的复制困境,分析了常规惯例复制和柔性惯例复制对知识转移的单独以及联合作用的关系悖论,对比分析作用机制在网络闭合性和环境不确定性约束下的权变性影响。以研发密集型企业为对象,运用多元回归分析进行实证检验。结果表明:网络闭合性和环境不确定性是惯例复制对知识转移的单独以及联合作用的权变条件;网络闭合性强化了常规惯例复制机制的促进作用,但限制了柔性惯例复制机制的效能发挥;环境不确定性削弱了常规惯例复制机制的促进作用,对柔性惯例复制机制的作用效果不显著;网络闭合性低或环境不确定性低时,两种惯例复制机制的联合作用相互补充,而网络闭合性高或环境不确定性高时,两种惯例复制机制相互替代。研究结论有助于揭示惯例复制的权变作用,对提升技术创新网络的知识转移效率具有重要意义。     

硫化锌纳米粒子的乳液合成

纳米材料被人们认为是新型的功能材料^[1]。作为过渡金属硫化物,硫化锌（ZnS)材料显示出许多特异光电性能,在许多领域有着广泛的应用^[2],因而一直被应用和研究。     

方兴未艾的纳米结构材料

介绍了纳米结构材料的结构,特性,制备方法以及广阔的应用前景。