纺织品中pH值的测定能力验证

为了了解国内纺织品检测机构对纺织品中pH值测定领域的整体水平,识别和掌握实验室存在的差异,加强纺织品检测机构的实验室能力建设,中国国家认证认可监督管理委员会(CNCA)组织了纺织品中pH值的测定能力验证活动,有16个省、市、直辖市的69个实验室参加,测试结果满意的实验室占78.26%.     

A porphyrin derivative containing 2-(oxymethyl)pyridine units showing unexpected ratiometric fluorescent recognition of Zn2+ with high selectivity

A porphyrin derivative (1), containing two 2-(oxymethyl)pyridine units has been designed and synthesized as chemosensor for recognition of metal ions. Unlike many common porphyrin derivatives that show response to different heavy metal ions, compound 1 exhibits unexpected ratiometric fluorescence response to Zn²⁺ with high selectivity. The response of the novel chemosensor to zinc was based on the porphyrin metallation with cooperating effect of 2-(oxymethyl)pyridine units. The change of fluorescence of 1 was attributed to the formation of an inclusion complex between porphyrin ring and Zn²⁺ by 1:1 complex ratio (K = 1.04 × 10⁵), which has been utilized as the basis of the fabrication of the Zn²⁺-sensitive fluorescent chemosensor. The analytical performance characteristics of the proposed Zn²⁺-sensitive chemosensor were investigated. The sensor can be applied to the quantification of Zn²⁺ with a linear range covering from 3.2 × 10⁻⁷ to 1.8 × 10⁻⁴ M and a detection limit of 5.5 × 10⁻⁸ M. The experiment results show that the response behavior of 1 to Zn²⁺ is pH-independent in medium condition (pH 4.0-8.0) and show excellent selectivity for Zn²⁺ over transition metal cations.     

穿心莲内酯硫酸酯化反应体系中四个新的衍生物的分离与表征

通过色谱方法, 从复杂的穿心莲内酯硫酸酯化反应体系中分离获得4个新的穿心莲内酯衍生物, 应用谱学方法进行了表征. 主要利用1H NMR, 13C NMR, DEPT, 1H-1H COSY, HSQC, HMBC及NOSEY等1D和2D NMR技术, 并通过与母体化合物NMR数据的对比分析, 鉴定这4个化合物分别为3,19-二羟基-8,11,13-赖百当三烯-15,16-内酯(1), 3-羟基-8,11,13-赖百当三烯-15,16-内酯-19-硫酸酯(2), 8,11,13-赖百当三烯-15,16-内酯-3,19-二硫酸酯(3), 3-羟基- 8(R)-12(S)-8(12)-环氧-13-赖百当烯-15,16-内酯-19-硫酸酯(4).     

Dielectric study on membrane adsorption and release: Relaxation mechanism and diffusion dynamics

Dielectric monitoring of the adsorption or release process of salicylic acid (SA) by chitosan membrane shows that the dielectric spectra of the chitosan membrane/ SA solution systems change regularly in the adsorption or release process. By analyzing the regularity, a new mechanism for the relaxations is proposed. The concentration polarization layer (CPL) caused by SA adsorption or release is confirmed to be essential for the dielectric relaxations. The changes of the spectra with time are explained by account of the relationship between CPL properties and dielectric strength. Based on this relaxation mechanism, a theoretical method can be established to calculate dynamical parameters of inner structure of the adsorption or release systems from their dielectric spectra. Therefore, dielectric spec- troscopy is demonstrated to be a promising method for estimating interfacial distribution of ionic sub- stances and their binding to membrane in a non-invasive way.     

Syntheses of (-)-oleocanthal, a natural NSAID found in extra virgin olive oil, the (-)-deacetoxy-oleuropein aglycone, and related analogues

Phenolic compounds extracted from extra virgin olive oil have attracted considerable recent attention. One of the components, (-)-oleocanthal (1), an inhibitor of the COX-1 and COX-2 enzymes, possesses similar potency as the NSAID ibuprofen. In this, a full account, we disclose the first- and now second-generation syntheses of both enantiomers of the oleocanthals, as well as the first synthesis of the closely related (-)-deacetoxy-oleuropein aglycone and a series of related analogues for structure activity studies. To demonstrate the utility of the second-generation synthesis, multigram quantities of (-)-oleocanthal were prepared in 10 steps (14% overall yield) from commercially available D-lyxose.     

Palladium nanocrystals bound by {110} or {100} facets: from one pot synthesis to electrochemistry

A facile one-pot tactic is developed for the selective synthesis of either rhombic dodecahedral or cubic Pd nanocrystals with high yields. By applying a mild cleaning process, we establish for the first time reasonable and distinct electrochemical features corresponding to {110} or {100} facet predominated Pd nanocrystals.     

硫酸化氧化锆固体超强酸

硫酸化氧化锆(SZ)是一种固体超强酸催化剂,它能高效催化异构化、烷化、酰化、环化、裂解、酯化和酯交换等多种类型的催化反应。1979年,日本科学家Hino和Arata发现SZ能在室温催化丁烷异构化反应,首次提出了SZ是一种酸性比100%浓硫酸还强一万倍的固体超强酸,从而引起了科学家们对SZ研究的浓厚兴趣。经过了三十多年发展,研究者们在SZ的合成、改性、表征和应用等方面取得了许多新的研究成果。本文综述了SZ几十年来的研究进展,内容主要包括SZ的合成方法,表面结构和酸性机理,研究者们对SZ性质的不同看法,SZ的改性及应用。     

Enantioselective concomitant creation of vicinal quaternary stereogenic centers via cyclization of alkynols triggered addition of azlactones

An asymmetric cyclization of alkynols triggered addition of azlactones catalyzed by a combined catalyst system consisting of a chiral gold phosphate and a phosphoric acid produces conformationally restricted amino acid precursors bearing vicinal quaternary stereogenic centers in high levels of stereoselectivity.     

ICP-MS法测定欧盟玩具新指令限制的17种可迁移元素

根据欧盟玩具安全新指令( 2009/48/EC)的要求,应用电感耦合等离子体质谱(ICP-MS)法测定玩具材料中硼、铝、铬、锰、钴、镍、铜、锌、砷、硒、锶、镉、锡、锑、钡、汞、铅17种可迁移元素含量,使用碰撞反应池技术消除某些多原子离子干扰.方法检出限为0.5～75μg/kg,加标回收率在85.4％～109％之间,相对...