交联网络和浓溶液中高分子链运动的NMR研究Ⅲ.质子自旋-晶格弛豫时间与凝胶和浓溶液体系中高分子链段的运动

用自旋－晶格弛豫时间（Ｔ１）研究了溶胀的交联聚丙烯酰胺－丙烯酸网络和线型聚苯乙烯溶液中质子的弛豫行为。交联网络中，随着交联度增大，Ｔ１ＣＨ／Ｔ１ＣＨ２的值由１．１７逐渐趋近于１；而线型聚苯乙烯溶液中，Ｔ１ＣＨ／Ｔ１ＣＨ２的值由最稀浓度下的１．７过渡到１。说明在交联网络中，交联度很低时，链段的运动已经相当受约束；但交联度很大时，充分溶胀的交联网络中链段运动仍有一定自由度。而在线型高分子浓溶液中，链段的运动严重受阻，导致自旋扩散效应非常完全，彻底平均掉了各质子间Ｔ１时间的差异。     

功能色素材料——苯重氮氨基偶氮苯类光度显色剂的研究

功能色素材料——苯重氮氨基偶氮苯类光度显色剂的研究罗小民周伟良孙培培吴斌才（华东师范大学化学系上海２０００６２）关键词光度显色剂离解电子光谱ＨＭＯ法中图分类号６２１．１３功能色素材料包括光致变色、电致变色、热致变色和压敏变色材料以及光度显色剂等。这些...     

精神分裂症患者头发5种元素含量变化及临床意义

采用原子吸收光谱法测定了９６例精神分裂症患者和１０１名正常对照组的头发Ｚｎ、Ｃｕ、Ｆｅ、Ｃａ、Ｍｇ元素含量。结果发现，精神分裂症患者头发ｎ和Ｍｇ元素含量明显低于对照组，而Ｃｕ、Ｆｅ和Ｃａ元素含量明显高于对照组。提示精神分裂症的发病，可能与Ｚｎ和Ｍｇ元素含量降低，Ｃｕ、Ｆｅ和Ｃａ元素含量升高有关。     

化学蒸气沉积硅氧化合物调变HZSM－5沸石的研究

本文研究了正硅酸乙酯分别在无胺法和有胺法制得的ＨＺＳＭ－５沸石上的沉积过程，并用吸附，ＮＨ３－ＴＰＤ及异丙醇探针反应等手段表征了沉积后的样品，发现沉积仅在外表面上进行，可使孔口变小但不影响孔道内性质，显示有对于二甲苯分子的择形吸附能力，且在甲苯甲醇烷基化反应和二甲苯异构化反应中表现出良好的择形催化性能．     

稀土在鼠肝中的物种分布

采用 ICP-MS、微量蛋白层析分离技术 ,研究了长时间、低剂量混合稀土及短时间、高剂量硝酸镧分别对大鼠及小鼠作用后 ,稀土在鼠肝中的代谢累积及其物种分布 .结果表明 ,鼠肝中各稀土含量随给药剂量的增加而增大 ,其累积速度大小顺序为 La>Ce>Nd>Pr;经柱层析分离未得到与稀土特异结合的鼠肝蛋白 ;稀土可与多种鼠肝蛋白 (包括多种重要的酶 )结合 ,在一定条件下 ,稀土与其结合蛋白可发生解离     

Determination of the Enantiomeric Purity of l-Carnitine and Acetyl-l-Carnitine by Chiral Liquid Chromatography

A chiral liquid chromatographic method for determination of the enantiomeric purity of both l-carnitine and acetyl-l-carnitine is described. Separation of the enantiomers of dl-carnitine and acetyl-dl-carnitine was achieved on a commercial chiral column (Chiralcel OD-R) after derivatization with (alpha-bromo)methyl phenyl ketone. Introduction of this lipophilic UV chromophoric group to the carnitine and acetylcarnitine molecules improved their retention, resolution, and UV detection. The mobile phase was 74:26 (v/v) 0.5 mol L^-1 sodium perchlorate–acetonitrile, pH 3.8, and the flow rate was 0.4 mL min^-1. Detection was performed at 235 nm. The method is selective and reliable for determination of the enantiomeric purity of bulk drug substances l-carnitine and acetyl-l-carnitine.     

Fluorimetric determination of ascorbic acid with o-phenylenediamine

A simple and sensitive fluorimetric method for the determination of ascorbic acid (AA) is described. The method is based on the condensation reaction between AA and o-phenylenediamine (OPDA) in the absence of the oxidant. The fluorescence intensity is measured at excitation and emission wavelengths of 360 and 430 nm, respectively. Under optimum condition, a linear relationship is obtained between the fluorescence intensity and the concentration of AA in the range of 0.05-40 μg ml⁻¹. The detection limit is 0.006 μg ml⁻¹, which is obviously lower than that of other fluorimetric methods reported.     

HPLC–MS Analysis of Isoniazid in Dog Plasma

A simple, rapid, and sensitive liquid chromatography–mass spectrometric (LC–MS) method was developed and validated for the determination of isoniazid in dog plasma. Plasma samples were deproteined with methanol and separated on a C₁₈ column interfaced with a single quadrupole mass spectrometer, using 0.1% formic acid–acetonitrile (91:9 v/v) as mobile phase. Detection was performed by positive electrospray ionization with selected ion monitoring at m/z 138 for isoniazid and 152 for entecavir maleate internal standard. Linearity was obtained over the range of 25–5,000 ng mL^?1, with a lower limit of quantification of 25 ng mL^?1. The intra- and inter-day precision was less than 2.7% in terms of relative standard deviation. Accuracy, expressed as relative error, ranged from ?2.0 to 8.0%. Plasma samples were analysed within 5 min. The method was successfully applied to the evaluation of the pharmacokinetics of isoniazid in dog plasma.     

吲哚乙酸与磷钼黄反应及其极谱分析的研究

在ＮＨ３－ＮＨ４Ｃｌ缓冲溶液中（ｐＨ＝９．５），吲哚乙酸与磷钼黄的还原产物在滴汞电极上于－１．１０Ｖ（ｖｓ．ＳＣＥ）处产生一灵敏的极谱波，该波波高与吲哚乙酸的浓度在１．０×１０－７－５．０×１０－６ｍｏｌ／Ｌ范围内成线性关系，检测下限为５．０×１０－８ｍｏｌ／Ｌ。如在上述还原产物中加入偶氮胭脂红Ｂ、孔雀绿、甲基紫等染料及聚乙烯醇，可使极谱波的灵敏度提高，使吲哚乙酸的浓度在５．０×１０－８－１．０×１０－６ｍｏｌ／Ｌ范围内与波高成线性关系，检测下限降低至１．０×１０－８ｍｏｌ／Ｌ。