流动注射-抑制化学发光测定多贝斯的方法研究

碱性条件下 ,多贝斯对铁氰化钾鲁米诺体系的化学发光有显著抑制作用 ,提出了一种用于多贝斯质量监测的流动注射 抑制化学发光分析方法。方法的线性范围为 1 .6× 1 0 - 5g/mL～ 2 .0× 1 0 - 7g/mL ;检测限 ( 3σ)为 4 4× 1 0 - 8g/mL ;RSD为 1 .5 % (c多贝斯=2 0× 1 0 - 7g/mL ,n =1 1 ) ;采样频率为 30 0次 /h。     

东莞市儿童血清中5种微量元素及钙含量的分析研究

测定了东莞市 1 3 89名儿童血清中锌 (Zn)、铁 (Fe)、铜 (Cu)、锰 (Mn)、铅 (Pb)及钙 (Ca)含量。结果分别为Zn (0 973± 0 2 3 8) μg/mL、Fe (1 1 0 1± 0 2 41 ) μg/mL、Cu (0 90 5±0 2 1 3 ) μg/mL、Mn (0 0 3 9± 0 0 2 0 ) μg/mL、Pb (0 0 5 3± 0 0 1 5 ) μg/mL及Ca (85 2 5 2± 1 4 795 )μg/mL,男女间没有显著差异。     

轻中度铅中毒儿童的干预治疗

为探讨轻中度铅中毒儿童的干预治疗的方法 ,将 96例血铅水平 10 0～ 4 0 0 μg/L的铅中毒儿童随机分成三组 :对照组为健康教育组 ;治疗A组为服钙组 ;治疗B组为混合组 :服食钙剂的同时 ,配合进行有关的健康教育。分别干预三个月后复查血铅水平。结果表明 ,三组儿童干预前后的血铅水平分别为 :对照组 (n =30 ) 2 0 6 0± 6 6 0 μg/L ,134 2± 4 2 9μg/L ,下降了 35% ;治疗A组(n =34) 2 0 8 5± 6 0 3μg/L ,12 4 0± 4 0 7μg/L ,下降了 4 1% ;治疗B组 (n =32 ) 2 2 5 9± 70 4 μg/L ,10 8 4± 33 8μg/L ,下降了 52 %。干预前各组间血铅水平没有差异 (P >0 0 5) ,而干预后对照组与治疗A组、对照组与治疗B组间比较 ,t分别为 0 970 (P >0 0 5)、2 6 36 (P <0 0 1) ,对照组与治疗B组之间有显著差异。提示健康教育及口服钙剂皆能明显降低轻中度铅中毒儿童的血铅水平 ,而两者同时配合进行 ,效果更加显著。     

毛细管区带电泳法测定粉针剂中头孢拉定的含量

用毛细管区带电泳法测定头孢拉定的含量 ,未涂层毛细管柱 (75 μm×48.5cm ,有效长度 40cm) ,电压 2 8kV ,检测波长 2 3 0nm ,温度 2 0℃ ,进样 5×1 0 3Pa× 3s。运行缓冲液为 2 5mmol/L硼砂缓冲液。方法的线性范围 3 1 .2 2μg/mL～ 749.2 8μg/mL ,检测限为 1 .1 7μg/mL。     

前列泰片在家兔体内的药代动力学研究

应用柱前衍生化HPLC法测定了以 4 %前列泰片悬浮液灌饲 (31mL/kg)家兔后 ,兔血浆中水苏碱 (Stachy drine)浓度 .结果表明水苏碱在家兔血中的经时变化符合二室模型 :峰浓度 (Cmax) 6 .2 9± 0 .84 μg/mL ;达峰时间(Tmax) 3.36± 0 .6 4h ;分布相半衰期 (T1/ 2α) 5 .35± 3.79h ;消除相半衰期 (T1/ 2 β) 32 .38± 2 4 .33h ;药时曲线下面积 (AUC)2 0 8.15± 118.4 μg/ (mL·h)     

流动注射化学发光法测定DL-酪氨酸

在甲醛存在下 ,高锰酸钾与DL 酪氨酸能够发生化学发光反应 ,产生很强的化学发光。据此采用流动注射技术 ,建立了一种测定DL 酪氨酸的化学发光分析法。方法的检出限为 2 .9× 1 0 - 8g/mL ,相对标准偏差为 1 .5 % ( 1 .0× 1 0 - 6g/mLDL 酪氨酸 ,n =1 1 ) ,线性范围为 1 .0× 1 0 - 7g/mL～ 5 .0× 1 0 - 6g/mL。     

以固体超强酸SO4^2-／ZrO2-Fe2O3催化合成醋酸异戊酯

以合成醋酸异戊酯为探针反应,筛选出制备固体超强酸SO2-4 /ZrO2- Fe2O3 (SZF -1 )的最佳工艺条件为:ZrOCl2·8H2O9. 7g, FeCl3·6H2O16. 2g, 常温陈化24h, 0. 5mol·L-1 H2SO4 (15mL·g-1 )浸泡5h, 550℃焙烧3h。以SZF 1为催化剂合成醋酸异戊酯的反应条件为:异戊醇200mmol, n(异戊醇)∶n(醋酸) =1. 0∶1. 3, SZF -1 1g(反应物总质量的3% ), 环己烷15mL, 回流反应3h, 酯化率93. 47%。催化剂连续使用6次后酯化率仍在70%以上。     

反相高效液相色谱法测定兔血清中拉莫三嗪的浓度及其动物药代动力学研究

 用反相高效液相色谱法测定了兔血清中抗癫痫药拉莫三嗪的浓度 ,以苯乙酮作内标 ,甲醇 磷酸二氢钾 ( 0 0 5mol/L ,pH 3 8)为流动相 ,经YWG ODS柱 ( 2 0 0mm× 3 6mmi d )分离 ,波长为 3 0 5nm的二极管阵列检测器检测 ,结果血药浓度在 0 2 5mg/L～ 5 0mg/L范围内线性良好 (r =0 9998) ,平均回收率为 93 78% ,标准误差为2 66% ,日内和日间RSD分别为 2 4 % (n =9)和 5 3 % (n =5 )。取家兔经胃给药 ( 2 5mg/kg) ,在设定时间抽血 ,测定动物药代动力学参数 ,经 3P87药代动力学程序包拟合 ,结果为Cmax=9 3 4 μg/mL ,t1/ 2 (Ke) =8 78h。     

微量元素对胎儿发育影响的临床研究

为了解小于胎龄儿的血锌、铜、铅的变化 ,对 3 8例小于胎龄儿 (其中 1 2例有先天缺陷 )进行了血锌、铜、铅三种微量元素检测 ,并与 3 1例健康足月适于胎龄儿比较。结果表明 ,3 8例小于胎龄儿血锌、铜、铅结果分别为 49 4± 1 9 88μmol/L、 1 0 7± 3 3 μmol/L、 1 5± 0 83 μmol/L ;与正常对照组 (分别为 62 3 9± 1 5 2 9μmol/L、 1 1 0 2± 1 73 μmol/L、 0 82± 0 3 9μmol/L)比较 ,血锌明显低于正常组 ,t=-2 88,P <0 0 1 ;血铅明显高于对照组 ,t =4 6,P <0 0 1 ,有显著性差异。两组血铜无明显差异。小于胎龄儿血锌降低 ,血铅增高 ,而且其先天性缺陷者占3 5 .5 8% ,证明胎儿的低锌高铅状态对其生长发育有重要影响。     

超高效液相色谱-串联质谱法同时测定动物组织中4种抗结核药物的残留量

建立了超高效液相色谱-串联质谱法同时测定鸡肉、牛肉、猪肉中4种抗结核药物残留量的检测方法。样品经酸化乙腈超声提取,HLB固相萃取柱净化,Luna~?C8柱(150 mm×2 mm,3μm)分离,电喷雾电离(ESI~+)和多反应监测(MRM)模式检测。结果表明,利福平、利福霉素、利福喷汀和利福布汀分别在0. 3"20. 0,0. 1"20. 0,0. 3"20. 0,0. 2"20. 0μg/L范围内呈良好线性,相关系数大于0. 99,定量限为0. 8"1. 2μg/kg。在1. 0,2. 0,10. 0μg/kg添加水平的平均回收率为66. 3%～104. 5%,日内相对标准偏差为4. 2%～13. 8%(n=6),鸡肉的日间相对标准偏差为4. 3%～13. 6%(n=3)。该法可用于动物组织中4种抗结核药物残留量的同时检测。     

多环芳二酐型聚酯亚胺膜的透气性能

多环芳二酐型聚酯亚胺膜的透气性能李悦生，丁孟贤，徐纪平（浙江大学高分子科学与工程研究所，杭州，３１００２７）（中国科学院长春应用化学研究所）关键词聚醚酰亚胺，聚酯酰亚胺，膜，透气性通常的聚酰亚胺加工性能较差，在芳环二酐的苯环间引入醚键等柔性基团后，其...     

Determination and study on residue and dissipation of benazolin-ethyl and quizalofop-p-ethyl in rape and soil

A QuEChERS (quick, easy, cheap, effective, rugged, and safe) method for the determination of benazolin-ethyl and quizalofop-p-ethyl in rape and soil by high-performance liquid chromatography-tandem mass spectrometry has been developed in this study. The residue and dissipation of benazolin-ethyl and quizalofop-p-ethyl in rape and soil were determined with the developed method. The half-lives of benazolin-ethyl in rape straw and soil were 3.7–5.1 days and 14.3–26.3 days, respectively. The half-lives of quizalofop-p-ethyl in rape straw and soil were 5.0-6.1 days and 0.3–9.7 days, respectively. The residue of benazolin-ethyl and quizalofop-p-ethyl in rapeseed and soil were below the detection limit (i.e., 0.5?mg?kg^?1, the maximum residue level of European Union for quizalofop-p-ethyl).     

微量元素与疾病诊断治疗的研究现状及展望

对国内外微量元素与疾病的关系及其诊断治疗的研究现状及研究动向进行了综述，包括：微量元素与地方病、癌肿、心血管病、糖尿病、眼病、神经系统病等。参考文献72篇。     

Ti-V基储氢合金及其氢化物的物相结构与组分优化设计

Ti-V基储氢合金在室温、常压下即可表现出良好的储氢特性,且质量储氢容量明显高于传统AB₅型储氢合金,从而在氢气的精制和回收、运输和储存及热泵等方面有较早的应用。 此外,在混合气体分离、核反应堆中处理氢的同位素、镍氢电池及燃料电池负极材料等方面也得到了广泛的研究与关注。 基于目前Ti-V基储氢合金的研究现状,概述了该类合金的优势、限制性因素(包括成因)及改性手段。 此外,为了进一步理解Ti-V基合金储氢机理、构建合金组分与储氢特性之间的对应关系,本工作重点围绕Ti-V基储氢合金及其氢化物的结构、组分优化设计展开综述,并对其未来研究方向做出展望。     

钒与糖代谢及糖尿病

微量元素钒作为生物体内必需元素，经证实有很重要的生理学功能，与机体糖代谢有十分密切的关系，且能降低糖尿病动物模型的高血糖，极有可能被开发为治疗糖尿病的药物。     

Ferrocene and ferrocenium modified clays and their styrene and EVA composites

In this work, ferrocene- and ferrocenium-containing salts were employed to modify montmorillonite. X-ray measurements show an increase in the interlayer spacing upon clay modification, which means that the larger and more organophilic cations were inserted into the gallery space of montmorillonite. Attempts to prepare nanocomposites of polystyrene and ethylene vinyl acetate copolymers lead to immiscible systems; the morphology of these systems was elucidated with TEM, XRD and cone calorimetry. The thermal stability of the composites is greater than that of the virgin polymer.     

Synthesis and Optical and Redox Properties of Symmetric and Asymmetric BODIPYs

Herein, we present the synthetic route and the photophysical, electrochemical as well as laser properties of novel red‐emitting boron‐dipyrromethenes (BODIPYs) bearing arylethyne moieties. Such functionality is added along the main axis of the chromophore leading to single‐ and double‐substituted derivatives. The relationship between the dye structure and the lasing properties is studied in detail with the help of the photophysical and electrochemical properties as well as quantum mechanical simulations. The asymmetric substitution of the parent dye induces inhomogeneities in the charge distribution, which leads to an overall loss of the fluorescence capacity, mainly in polar media. Such non‐radiative deactivation processes can be softened by decreasing the electron‐donor ability of the substituent or even avoided by symmetrical substitution. Thus, grafting of the arylethyne moieties at the longitudinal axis of the indacene core results in an effective strategy to develop red‐edge BODIPYs with highly efficient and photostable laser emission.     

Synthesis of Tyrosol and Hydroxytyrosol Glycofuranosides and Their Biochemical and Biological Activities in Cell-Free and Cellular Assays

Tyrosol (T) and hydroxytyrosol (HOT) and their glycosides are promising candidates for applications in functional food products or in complementary therapy. A series of phenylethanoid glycofuranosides (PEGFs) were synthesized to compare some of their biochemical and biological activities with T and HOT. The optimization of glycosylation promoted by environmentally benign basic zinc carbonate was performed to prepare HOT α-L-arabino-, β-D-apio-, and β-D-ribofuranosides. T and HOT β-D-fructofuranosides, prepared by enzymatic transfructosylation of T and HOT, were also included in the comparative study. The antioxidant capacity and DNA-protective potential of T, HOT, and PEGFs on plasmid DNA were determined using cell-free assays. The DNA-damaging potential of the studied compounds for human hepatoma HepG2 cells and their DNA-protective potential on HepG2 cells against hydrogen peroxide were evaluated using the comet assay. Experiments revealed a spectrum of different activities of the studied compounds. HOT and HOT β-D-fructofuranoside appear to be the best-performing scavengers and protectants of plasmid DNA and HepG2 cells. T and T β-D-fructofuranoside display almost zero or low scavenging/antioxidant activity and protective effects on plasmid DNA or HepG2 cells. The results imply that especially HOT β-D-fructofuranoside and β-D-apiofuranoside could be considered as prospective molecules for the subsequent design of supplements with potential in food and health protection.     

Conformations and steric and stacking interactions of trisubstituted ureas and thioureas with alkyl and phenyl groups

The monomeric ν(N—H) vibrations of various trisubstituted ureas of the R₂UPh type and -thioureas of the R₂TUPh type have been studied. The trans—out isomerism in the former and the trans—out—cis isomerism in the latter are discussed from the point of view of steric effect. The monomeric ν(N—H) vibrations of RPhUPh and RPhTUPh are also examined. The single band appearing in the spectrum of both ureas is characteristic of the cis form; this suggests the existence of phenyl—phenyl interaction (the stacking interaction proposed by Galabov et al. [10]). Behavior of ν(N—H) vibrations at several concentrations is shown to be clearly different in the three forms (trans, out and cis). The presence of the cis form is confirmed by solvent effect experiments.