高效毛细管电泳间接紫外检测血浆中钾、钙、镁

用高效毛细管电泳法,在pH 5.5的缓冲介质中用酒石酸作为络合剂,使血浆中钾、钠、钙、镁4种阳离子达到很好分离,用咪唑作为背景试剂进行了紫外检测.对电泳分离及紫外检测的各分析条件(包括背景缓冲溶液的pH值,咪唑溶液的浓度及酒石酸溶液的浓度等)作了试验并予以优化,上述4种离子的相互分离在4.5 min内顺利完成.文中给出了K 、Ca 、Mg2 的线性回归方程,其相关系数在0.998 4～0.999 4之间,证明了在各离子的峰面积与其浓度之间呈线性关系,3种离子的检出限(S/N=3)依次为0.20,0.12,0.06 mg·L-1.用迁移时间检测和用峰面积检测所得的RSD值(n=6)依次小于0.76%和2.83%.由于钠离子的吸收峰与系统峰重叠,钠的测定无法进行.回收率试验的结果在95.3%至104.2%.     

温敏性聚合物复合体系低临界溶解温度的研究

研究了温敏性N-异丙基丙烯酰胺的均聚物(PNIPAm)及其共聚物P(NIPAm-co-KYD)与十六烷基三甲基氯化铵(CTAC)、乙二胺四乙酸(EDTA)、盐等复配体系的低临界溶解温度(LCST)的变化规律。单因素复配体系中,wEDTA为0.1%时,体系LCST从33℃降低到25℃,增大到0.2%时,LCST下降趋于缓慢;wCTAC在0.5%-3.0%范围内,LCST先上升后下降,但wCTAC在0.5%-1.0%内相转变很不明显,超过1.5%后相转变又趋于明显;而无机盐能使体系LCST线性下降;多因素复配体系中LCST变化较缓和,易于控制且相转变现象明显。     

Tris(2,2''''-bipyridyl)ruthenium(Ⅱ) electrochemiluminescence (ECL) enhanced by rutin on platinum electrode

Ru(bpy)_(3~(2 )) electrochemiluminescence (ECL) was applied to determination of rutin. ECL intensity of Ru(bpy)_(3~(2 ))could be enhanced in the presence of rutin in basic solution on platinum electrode. At pH 9.9, light emission intensity was found to be linear with rutin in the range of 1-50 mmol/L.     

胶原纤维固化黑荆树单宁吸附V(V)的研究

研究了胶原纤维固化黑荆树单宁对V(V)的吸附。采用不同温度、pH值等条件进行吸附研究,并进一步探讨了固化黑荆树单宁的吸附动力学和吸附柱动力学及其吸附机理。结果表明,该材料对V(V)的吸附平衡符合Freund lich方程,温度对吸附平衡的影响不明显;吸附动力学可用拟二级速度方程来描述,该材料同时具有良好的柱动力学特性;V(V)的吸附过程可能存在三个反应,即V(V)与吸附剂之间发生氧化还原反应生成V(IV),V(IV)和-COOH之间发生离子交换反应,以及V(IV)与单宁的邻位羟基发生螯合。     

水解聚合铝溶液中Al30形态的研究

水解聚合铝形态一直是分析、催化、土壤、地球化学、新材料、环境科学和生物毒理学等众多领域研究的前沿和热点。Keggin 结构的Al₃₀ 形态是迄今为止发现的电荷最高的水解铝聚合阳离子,具有独特的分子结构和纳米分子尺寸,它对催化化学、新型功能材料、高效絮凝剂的开发以及铝的水解聚合转化规律研究具有重要意义。本文主要论述了Al₃₀形态的形成、形态分析方法、结构模型以及形成机理等方面的最新研究进展,并对水解聚合铝溶液的研究发展趋势进行了展望。     

Determination of sulfite in Oriental herbal medicines

Sulfite was detected in 7 varieties of Oriental herbal medicines (Pueraria radix, Zingiberis rhizoma, Platycodon radix, Adenophora radix, Pinellia tuber, Astragalus radix, and Paeonia radix) on the Korean market. Sulfiting of commercial Oriental herbal medicines by fumigation with burning bituminous coal was simulated, and the accumulation of sulfite was investigated by using fresh Platycodon radix roots obtained from a growing field. The sulfite level reached a plateau in 9 h, and the maximum sulfite level found by the Monier-Williams (MW) method (AOAC 990.28) was 1020 ppm. The sulfite content in the simulated Platycodon radix sample determined by alkali extraction followed by ion-exclusion chromatography with electrochemical detection (AOAC 990.31) was approximately 17% lower on average than the MW results. Free-sulfite levels determined by acid extraction and ion-exclusion chromatography with electrochemical detection were between 19 and 49% of the MW results. The advantages of different methods for sulfite determination and the significance of the results are discussed.     

Synthesis of gramicidin S and its analogues via an on-resin macrolactamization assisted by a predisposed conformation of the linear precursors

A simple and efficient preparation of gramicidin S and its analogues is described. It involves solid-phase peptide synthesis and on-resin macrolactamization without side chain protection, affording cyclic products in high yield and high purity. The high specificity of the cyclization reaction was shown to originate in the formation of a pre-organized conformation of the linear biosynthetic precursor of gramicidin S. This facile method will provide convenient access to the analogues of the natural product for functional optimization to counter microbial resistance.     

异维A酸新木脂素酯的合成与表征

以香草醛(或对羟基苯甲醛)和丙二酸为原料,经Knoevenagel反应、酯化、氧化银为氧化剂的自由基仿生氧化偶联反应合成了新木脂素3a,3b。3a,3b分别与异维A酸酯化,合成了两种新型的异维A酸新木脂素酯4a和4b。用1H NMR,IR和MS对它们的结构进行了表征。研究了异维A酸酯的反应机理。     

Utilization of a spiropyran derivative in a polymeric film optode for selective fluorescent sensing of zinc ion

Spiropyrans are the most studied families of func- tional materials due to their reversible structural con- version in response to external optical, chemical, and thermal stimulation[1]. Irradiation with ultraviolet light causes formation of an extended π-conjugation open form (merocyanine form) by heterolytic cleavage of the C (spiro)-O bond, which generates an intense ab- sorption in the visible region. Under the irradiating of visible light, the opened form will come back to the closed spi…