茂基稀土胺化物与异氰酸正己酯的反应-{(MeC5H4)2Yb[OC(NPh2)N(n-hexyl)]}2的合成及表征

茂基稀土胺化物(MeCp)2YbNPh2(THF)与异氰酸正己酯(n-HexylNCO)按11摩尔比反应, 分离出产物{(MeC5H4)2Yb[OC(NPh2)N(n-hexyl)]}2. 产物经元素分析和核磁共振表征, 并测定了其晶体结构. 配合物属三斜晶系, R-3空间群, 晶胞参数为a=2.9533(11) nm, b=2.9533(11) nm, c=1.5873(6) nm, V=11.9896(80) nm3, Z=9, Dc=1.562 mg·m-3, μ=3.536 mm-1 (Mo Kα), F(000)=5670, R=0.034, Rw=0.064. 该化合物具有二个对称氧桥的双分子结构, 并存在着由氮原子向中心金属镱分子内配位而形成的三环骨架, 中心金属镱的配位数是九, 整个分子呈中心对称.     

电极条件对硫酸介质中电解还原提纯镱过程的影响

研究了以钌铱钛合金网和汞分别为阳、阴电极, 在无气氛保护条件下, 采用电解还原方法从铥、镱、镥硫酸盐溶液中分离提纯镱的过程. 讨论了在8 V恒电压时的电极间距、位置, 以及阴、阳极表面积对电解过程中的电流、还原率影响. 优化了电解还原过程, YbSO4产品的纯度稳定达到99.5%以上, 一次收率可达80%;提镱后母液中的铥和镥被富集4倍以上, 其中Lu含量高于50%, 十分有利于后续铥/镥分离.     

Rapid determination of acetone in human blood by derivatization with pentafluorobenzyl hydroxylamine followed by headspace liquid-phase microextraction and gas chromatography/mass spectrometry

In the current work, a simple, rapid, accurate and inexpensive method was developed for the determination of acetone in human blood. The proposed method is based on derivatization with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA), followed by headspace liquid-phase microextraction (HS-LPME) and gas chromatography/mass spectrometry (GC/MS). In the present method, acetone in blood samples was derivatized with PFBHA and acetone oxime formed in several seconds. The formed oxime was enriched by HS-LPME using the organic solvent film (OSF) formed in a microsyringe barrel as extraction interface. Finally, the enriched oxime was analyzed by GC/MS in electron ionization (EI) mode. HS-LPME parameters including solvent, syringe plunger withdrawal rate, sampling volume, and extraction cycle were optimized and the method reproducibility, linearity, recovery and detection limit were studied. The proposed method was applied to determination of acetone in diabetes blood and normal blood. It has been shown that derivatization with HS-LPME and GC/MS is an alternative method for determination of the diabetes biomarker, acetone, in blood samples.     

析相光度法测定铜（Ⅱ）的研究

本文研究了Ｃｕ（Ⅱ）－ＰＥＧ（聚乙二醇－２０００）－Ｚｉｎｃｏｎ（锌试剂）－（ＮＨ４）２ＳＯ４体系的析相光度法并应用于测定Ｃｕ（Ⅱ）。最宜酸度为ｐＨ５．５～８．５（ＫＨ２ＰＯ４－Ｋ２ＨＰＯ４）缓冲溶液）其络合物的最大吸收位于６１０ｎｍ，表观摩尔吸光系数为４．０×１０＾４Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，Ｃｕ（Ⅱ）浓度在０～１．５ｍｇ／Ｌ范围内服从比尔定律，铜与Ｚｉｎｃｏｎ形式组成为１：２的稳定的蓝色络     

Studies on the Physicochemical Properties, Structure and Antitumor Activity of an Oligosaccharide Homologue SnS-2 from the Root of Scrophularia ningpoensis Hemsh

An oligosaccharide homologue named SnS-2 was isolated from the root of Scrophularia ningpoensis Hemsl.SnS-2 was purified by means of gel-permeation chromatography and ion-exchange chromatography. Its physicochemical properties, including carbohydrate content and molecular weight were determined. The structure of SnS-2 was elucidated by chemical methods along with ^1H and ^13C NMR spectroscopy, including two-dimensional DQCOSY and H-detected ^1H, ^13C HMQC experiments. These results show that SnS-2 possesses a backbone consisting of terminal α-Galp-(1→, α-Galp-(1→6), α-Glcp-(1→6) and nonreducing end β-Fruf-(2→. The bioactive assay showed that it could inhibit the growth of Lewis pulmonary carcinoma implanted in mice.     

压力流驱动电色谱分析方法及其若干色谱行为

压力流驱动电色谱分析方法是一种新型色谱技术。它组合了ＨＰＬＣ和电泳两种技术，为分离提供了更多可控制的因素。介绍了压力流驱动电色谱的装置和毛细管电色谱柱的装置方法，从理论上讨论了影响电色谱分离的因素并用实验数据加以证明。最后尝试性地将电色谱法用于测定香蕉样品中萨索啉（Ｓａｌｓｏｌｉｎｏｌ）等的含量。     

Synthesis and antiangiogenic activities of 5-amino-1,3-dihydro-1, 3-dioxo-2H-isoindole-2-propanoic acid derivatives

Based on the structure-activity relationships and antiangiogenic mechanism of RGD-containing peptides,a series of 5-amino- 1,3-dihydro-1,3-dioxo-2H-isoindole derivatives were synthesized.The structures were characterized by ~1H NMR,MS and elementary analysis.There ability to inhibit angiogenesis were evaluated by chick embryo chorioallantoic membrane assay at 10~(-5) mol/L.Compounds 7a and 7b displayed obvious antiangiogenic activity.     

分析信号处理方法的比较研究

研究了高效液相色谱－火焰原子吸收光谱联用系统分析信号处理方法，比较了各种处理方法的优缺点，用积分与适应平滑法综合处理色谱峰分析信号，不仅能有效地消除噪声，而且能使分析信号得到加强，以测定镍为例，经积分与适应平滑法综合处理后，检出限改善了２．７倍。     

Poly[[aqua­tetra­imidazole­di‐μ‐phthalato‐dicopper(II)] monohydrate]

The title complex, {[Cu₂(C₈H₄O₄)₂(C₃H₄N₂)₄(H₂O)]·H₂O}_n, is a three‐dimensional polymer formed through bridging by phthalate dianions of two different Cu^II cations and a network of O(N)—H⋯O hydrogen bonds. The Cu—O and Cu—N inter­action distances are in the ranges 2.0020 (16)–2.4835 (17) and 1.968 (2)–1.9855 (19) Å, respectively. The structure is composed of alternating polymer chains parallel to the c axis, with a shortest Cu⋯Cu distance of 6.3000 (5) Å.