高效液相色谱法测定婴幼儿配方米粉和乳粉中 烟酸和烟酰胺含量

目的建立高效液相色谱法测定婴幼儿配方米粉和乳粉中烟酸和烟酰胺的提取分析方法。方法婴幼儿配方米粉和乳粉以10%甲醇+0.1%磷酸水溶液为提取液,超声提取,离心去除杂质,取上清液并用微孔滤膜(0.2μm)过滤,以十二烷基硫酸钠(SDS)缓冲液-乙腈(74:26,V:V)为流动相,利用高效液相色谱分析,外标法定量。结果该方法经过验证在0.20~30 mg/L质量浓度范围内,线性关系良好,烟酸、烟酰胺相关系数大于0.999,回收率在99.07%~110.33%之间,RSD小于5%。结论与现行标准方法相比,本方法前处理方法简单、基质干扰小,测定结果准确度高、重现性好,尤其对米粉中烟酸及烟酰胺的提取效率更高,可用于婴幼儿配方米粉和乳粉中烟酸及烟酰胺含量测定的快速、批量分析。     

Brønsted-acid-catalyzed asymmetric multicomponent reactions for the facile synthesis of highly enantioenriched structurally diverse nitrogenous heterocycles

Optically pure nitrogenous compounds, and especially nitrogen-containing heterocycles, have drawn intense research attention because of their frequent isolation as natural products. These compounds have wide-ranging biological and pharmaceutical activities, offering potential as new drug candidates. Among the various synthetic approaches to nitrogenous heterocycles, the use of asymmetric multicomponent reactions (MCRs) catalyzed by chiral phosphoric acids has recently emerged as a particularly robust tool. This method combines the prominent merits of MCRs with organocatalysis, thus affording enantio-enriched nitrogenous heterocyclic compounds with excellent enantioselectivity, atom economy, bond-forming efficiency, structural diversity, and complexity. In this Account, we discuss a variety of asymmetric MCRs catalyzed by chiral phosphoric acids that lead to the production of structurally diverse nitrogenous heterocycles. In MCRs, three or more reagents are combined simultaneously to produce a single product containing structural contributions from all the components. These one-pot processes are especially useful in the construction of heterocyclic cores: they can provide a high degree of both complexity and diversity for a targeted set of scaffolds while minimizing the number of synthetic operations. Unfortunately, enantioselective MCRs have thus far been relatively underdeveloped. Particularly lacking are reactions that proceed through imine intermediates, which are formed from the condensation of carbonyls and amines. The concomitant generation of water in the condensation reaction can deactivate some Lewis acid catalysts, resulting in premature termination of the reaction. Thus, chiral catalysts typically must be compatible with water for MCRs to generate nitrogenous compounds. Recently, organocatalytic MCRs have proven valuable in this respect. Br?nsted acids, an important class of organocatalysts, are highly compatible with water and thereby offer great potential as chiral catalysts for multicomponent protocols that unavoidably release water molecules during the course of the reaction. We present a detailed investigation of several MCRs catalyzed by chiral phosphoric acids, including Biginelli and Biginelli-like reactions; 1,3-dipolar cycloadditions; aza Diels-Alder reactions; and some other cyclization reactions. These approaches have enabled the facile preparation of 3,4-dihydropyrimidinones, pyrrolidines, piperidines, and dihydropyridines with high optical purity. The synthetic applications of these new protocols are also discussed, together with theoretical studies of the reaction transition states that address the regio- and stereochemistry. In addition, we briefly illustrate the application of a recently developed strategy that involves relay catalysis by a binary system consisting of a chiral phosphoric acid and a metal complex. This technique has provided access to new reactions that generate structurally diverse and complex heterocycles. Enantioselective organocatalytic MCRs remain a challenge, but we illustrate success on several fronts with chiral phosphoric acids as the primary catalysts. Further progress will undoubtedly provide even better access to the chiral nitrogen-containing heterocycles that are not only prevalent as natural products but also serve as key chiral building blocks in organic synthesis.     

平煤天安股份六矿主斜井皮带机电控系统改造

针对主斜井钢丝绳牵引胶带输送机存在电控系统的老化问题,提出优化改造、更新设备,提高系统的可靠性、安全性、灵敏性等问题,实现了钢丝绳牵引胶带输送机原电控系统的自动控制。     

Numerical investigation on Rayleigh-Bénard-Marangoni flow of water near the maximum density in cylindrical pools with large aspect ratios

We report a set of direct numerical simulation results on Rayleigh-Bénard-Marangoni (R-B-M) flow of cold water in the cylindrical pools. The heat transfer between the free surface and the environment is considered. The aspect ratio Г of the cylindrical pool varies from 2 to 8. Rayleigh (Ra) and Biot (Bi) numbers are respectively confined in Ra ≤ 10⁴ and 0 < Bi ≤ 50. The flow onset critical Ra is determined and the influences of Bi and the density inversion parameter (Θ_m) on the critical Ra are analyzed. The primary bifurcation flow structures of R-B-M flow are shown and the evolution of the flow structures with Ra and Bi at different Θ_m is observed. Furthermore, the heat transfer ability is estimated by Nusselt number. The results indicate that the critical Ra of the flow onset increases with increasing Bi and Θ_m. But it decreases with the increase of Г. The primary bifurcation pattern is multicellular flow. With increasing Г, the number of flow cells in multicellular flow increases fast. With increasing Ra, the up-triangular and up-quadrilateral flow structures appear at Г = 4, and finally transits to the up one-torus. With increasing Ra and Г, and decreasing Θ_m, average Nusselt number increases monotonically. However, with increasing Bi, it first increases, and then decreases.