植物生物分子的电分析化学研究Ⅷ.秋水仙碱的微分脉冲极谱行为及分析应用

秋水仙碱是近年来新发现的有前途的抗癌植物有效成分。秋水仙碱的测定方法,如容量滴定法^[1]、电位滴定法^[2]、紫外分光光度法^[3]、荧光分析法^[4]和高效液相色谱法^[5]等,手续均不太简便。电化学分析研究秋水仙碱主要有阳极伏安法^[6]和交流极谱法^[7],前者因使用固态电极,重现性较差。后者用非水溶剂作介质,灵敏度不高。     

二苯并噻吩及其氧化物与离子液体相互作用的理论研究

采用密度泛函理论方法比较了DBT/DBTO₂和[BMIM]⁺[PF₆]^-/[BMIM]⁺[BF₄]^-的相互作用。对最稳定的[BMIM]⁺[PF₆]^-、[BMIM]⁺[PF₆]^--DBT、[BMIM]⁺[PF₆]^--DBTO₂、[BMIM]⁺[BF₄]^-、[BMIM]⁺[BF₄]^--DBT、[BMIM]⁺[BF₄]^--DBTO₂进行了NBO和AIM分析。结果表明,DBT和[BMIM]⁺[PF₆]^-/[BMIM]⁺[BF₄]^-中的咪唑环彼此相互平行,NBO和AIM分析表明它们之间发生了π-π相互作用。H1'和H9'形成的F…H氢键有利于π-π堆积作用的形成。DBTO₂倾向于趋近C2-H2和甲基基团形成O…H相互作用;DBTO₂优先吸附在[BMIM]⁺[PF₆]^-/[BMIM]⁺[BF₄]^-。在模拟油中,[BMIM]⁺[PF₆]^-和[BMIM]⁺[BF₄]^-离子液体对DBTO₂的萃取能力大于DBT,其原因是可能是DBTO₂具有较大的极性和O…H与F…H的氢键作用。     

硝基磺酚C光度法测定蛋白质的研究

蛋白质的定量分析是生化研究、临床化验和食品检验等领域经常涉及的内容.以有机小分子作光谱探针测定蛋白质,如甲基橙^[1,2]、考马斯亮蓝G-250^[3]、溴酚蓝^[4]、溴甲酚绿^[5]和偶氮胂Ⅲ^[6]等已得到研究.     

阴离子碳菁染料的合成与聚集动力学研究

自从1938年,Scheibe^[1]发现了菁染料聚集体中的能量传递现象,人们对菁染料的聚集行为展开了大量的研究^[2,3].由于菁染料聚集体对乳剂具有特殊的增感作用,人们主要研究聚集体在乳剂中的增感机理^[4,5]以及菁染料聚集的溶剂效应与浓度效应^[6]等,而对于菁染料聚集的动力学行为研究较少.     

静电纺丝法制备NiO纳米纤维及其表征

纳米级NiO因具有优良的催化和热敏等性能而被广泛用于催化剂^[1]、电池电极^[2,3]、光电转化材料^[4～6]、电化学电容器^[7～8]等诸多方面.迄今,已成功地制备出N iO的纳米颗粒^[9]、纳米线^[10]及纳米薄膜^[11],但是对于具有准一维结构的NiO纳米纤维的制备及性能研究尚未见报道.     

零电流示波电位滴定盐酸异丙嗪

盐酸异丙嗪是一种较重要的抗组胺药,现行的分析标准为非水滴定法^[1],此外尚有分光光度法^[2]、伏安法^[3]、电极法^[4]、液相色谱法^[5]和流动注射分析法^[6]等。本文将高鸿提出的零电流示波电位滴定法^[7]中的铂片电极修饰一层含四苯基硼酸-异丙嗪电活性物质的PVC膜,使电极对异丙嗪产生响应,可用于四苯基硼酸钠直接滴定异丙嗪的终点指示。     

四(4-重氮基苯基)卟啉的合成及其与聚苯乙烯磺酸钠自组装的研究

卟啉是一类重要的功能性小分子染料,近年来,在光化学治疗^[1,2]、光电转换^[3,4]、传感元件^[5]、烯烃环氧化催化剂^[6]和光敏化剂^[7]等方面的研究与应用引起了人们的广泛注意.通过两亲卟啉分子衍生物,或带有负电荷的卟啉衍生物,特别是带磺酸基的卟啉分子与正离子聚电解质自组装,制备带有卟啉结构单元的LB膜和自组装膜已有很多报道^[8～14].     

有机卤化合物中卤素的离子选择性电极的快速微量分析

近年来,离子选择性电极已应用于有机氯、溴^[1-3]及碘^[4]的微量分析。但在电位滴定中,水介质的终点不明显^[5-6],非水介质用的乙酸^[1,2]有刺激性,而1,4-二氧环^[3]已烷则价太贵。     

微波消解-微波等离子体炬原子发射光谱法测定无铅汽油中痕量铅的研究

四乙基铅作为一种良好的抗爆添加剂,曾广泛用于汽油生产中,但由于四乙基铅有很强的毒性,目前国际上已停止生产和使用车用含铅汽油,因此在生产车用无铅汽油时严格控制和准确测定铅的含量十分必要.迄今,测定汽油中铅含量的常用方法是铬酸盐容量法^[1]、一氯化碘法^[2]、X射线光谱法^[3]、分光光度法^[4,5]、原子吸收光谱法^[6]和等离子体光谱法^[7].这些方法或操作烦琐,测定时间较长^[4],或灵敏度低^[1～3],或测定误差较大,且在测试中需使用毒性较大的四乙基铅^[5],或所需的氯化甲基三辛基铵不易购买^[6],或处理过程繁琐,且仪器设备昂贵^[7].因此,建立一种简便、快速、灵敏、准确和无毒副作用的测定无铅汽油中痕量铅的方法已显得十分迫切.近年来发展的微波等离子体炬原子发射光谱法^[8]已有商品化仪器问世^[9].本文利用微波等离子体炬原子发射光谱仪研究了无铅汽油中痕量铅的测定方法,并提出用微波消解法预处理无铅汽油样品,将微波消解技术与微波等离子体炬原子发射光谱法相结合,建立了简便、快速、灵敏、准确和无污染的测定无铅汽油中痕量铅的新方法.     

dl-萘普生的简便合成及其光学异构体的拆分

萘普生(S)-(+)-2-(6-甲氧基-2-萘基)丙酸(1)是一种新型非甾体抗菌消炎药物,临床应用十分广泛,疗效显著^[1]。其分子结构中有一个不对称碳原子,S体比R体的药理作用要强28倍^[3]。     

Determination of transition metal ions in tobacco as their 2-(2-quinolinylazo)-5-dimethylaminophenol derivatives using reversed-phase liquid chromatography with UV-VIS detection

This paper reports the utilization of solid-phase extraction and the reversed-phase high-performance liquid chromatography for the determination of six important transition metal ions: iron, cobalt, nickel, copper, zinc and manganese in tobacco with 2-(2-quinolinylazo)-5-dimethylaminophenol (QADMAP) as chelating reagent. Iron, cobalt, nickel, copper, zinc and manganese ions react with QADMAP to form colored chelates in the medium of acetic acid-sodium acetate buffer solution (pH 4.0). These chelates can be enriched by solid-phase extraction with Waters Sep-Pak-C18 cartridge, and eluted the retained chelates from cartridge with tetrahydrofuran. The chelates were separated on a Waters Nova-Pak-C18 column (150x3.9 mm, 5 microm) by gradient elution with methanol (containing 0.5% of acetic acid) and 0.05 mol/l pH 4.0 acetic acid-sodium acetate buffer solution as mobile phase at a flow-rate of 0.5 ml/min. The detection limits of iron, cobalt, nickel, copper, zinc and manganese are 10, 12, 8, 13, 17 and 22 ng/l, respectively. This method had been applied to the determination of iron, cobalt, nickel, copper, zinc and manganese in tobacco with good results.     

Determination of Manganese (II) in Foodstuffs by β-Cyclodextrin Polymer Phase Spectrophotometry with 1-(2-Pyridylazo)-2-naphthol

The chromogenic agent, 1-(2-pyridylazo)-2-naphthol (PAN) was included in g -Cyclodextrin polymer ( g -CDP) and the modified polymer of inclusion of PAN ( g -CDP-PAN) was obtained. Based on the fact that g -CDP-PAN can adsorb Mn (II) in solution to form Mn (II)-PAN complex, a sensitive and selective solid phase spectrophotometric method for the determination of trace amounts of Mn (II) has been developed. The maximum absorbance of Mn (II)-PAN complex in g -CDP was at 514 nm. The working range of the calibration graph was 2-12 w g of Mn (II). The interference of molybdenum, lead, cobalt, chromium, iron, nickel, zinc, tin, cadmium, and copper that form colored species with PAN in the polymer phase was investigated. The method was applied to the determination of Mn (II) in black rice and tea samples. A new method for the determination of trace amounts of manganese by polymer phase spectrophotometry is described. Manganese reacted with 1-(2-pyridylazo)-2-naphthol (PAN) that was included in a g -cyclodextrin polymer. The absorbance of the colored polymer, packed into a 5 mm quartz cell, was determined directly at 514 nm. The proposed method was applied to the determination of manganese in black rice and tea samples.     

火焰原子吸收法测定竹荪中的微量元素

使用灰化法处理样品,火焰原子吸收光谱法测定了竹荪中的钾、钙、钠、镁、铁、锰、铜、锌的含量。结果显示,竹荪中含有丰富的铁、锰、铜、锌4种人体必需微量元素。加标回收率为93.2%~103.2%,该法测定快速、简单,结果满意。     

Study on Determination of Six Transition Metal Ions in Biological Samples by SPE and RP‐HPLC

This paper reports the utilization of solid phase extraction and the reversed‐phase high‐performance liquid chromatography (RP‐HPLC) for the determination of six transition metal ions (iron, cobalt, nickel, copper, zinc and manganese) in biological samples. The samples were digested by microwave digestion. The iron, cobalt, nickel, copper, zinc and manganese ions in the digested samples can react with 2‐(2‐quinolinylazo)‐5‐diethylaminophenol (QADEAP) to form colored chelates in pH 4.0 acetic acid‐sodium acetic buffer solutions and cetyl trimethylammonium bromide (CTMAB) medium. These chelates were enriched by solid phase extraction with C₁₈ cartridge. Then the chelates were separated on a Waters Nova‐Pak‐C₁₈ column (3.9 × 150 mm, 5 μm) by gradient elution with methanol (containing 0.5% of acetic acid and 0.1% of CTMAB) and 0.05 mol/L pH 4.0 acetic acid‐sodium acetic buffer solution (containing 0.1% of CTMAB) as mobile phase at a flow rate of 0.5 mL/min. The detection limits of iron, cobalt, nickel, copper, zinc and manganese are 3 ng/L, 4 ng/L, 2 ng/L, 4 ng/L, 8 ng/L, 10 ng/L, respectively. This method was applied to the determination of iron, cobalt, nickel, copper, zinc and manganese in biological samples with good results.     

火焰原子吸收光谱法测定茶叶中的锰

介绍悬浮液进样-次灵敏线火焰原子吸收光谱法测定茶叶中的锰的方法。以琼脂为悬浮剂，将茶叶样品均匀、稳定地悬浮于琼脂溶胶中，直接喷入空气-乙炔火焰中，利用锰280.1nm次灵敏线，以工作曲线或标准加入法测定锰的含量，方法简便、快速，用于测定茶叶和桃叶样品中的锰，结果准确。     

主成分-偏最小二乘分光光度法同时测定饲料中的痕量铁、锰、铜、锌

痕量Fe^3＋、Mn^2＋、Cu^2＋、Zn^2＋与2-（5-溴-2-吡啶偶氮）．5-二乙氨基苯酚（5-Br-PADAP）和对．（1,1,3,3．四甲基丁基）苯基醚（Triton X-100）在pH8．3发生高灵敏显色反应,所形成的三元胶束络合物的吸收光谱严重重叠。本文采用主成分-偏最小二乘法（PC—PLS）辅助分光光度法成功地测定了合成试样及饲料中上述4种痕量组分。结果表明,PC—PLS法是化学计量学法中一种可适用于基体较复杂的实际试样中痕量组分同时分光光度测定的优良的多元计算方法。     

FAAS法连续分析测试电池锌粉中镁铁铜铅锰

提出了运用FAAS法连续分析测试电池锌粉中Mg、Fe、Cu、Pb、Mn的含量,给出了Mg、Fe、Cu、Pb、Mn最佳测定条件及线性范围,在测定中对样品中的干扰因素进行了综合考虑.方法具有很好的灵敏度和重现性,步骤简单、操作容易、干扰少.测定样品Mg、Fe、Cu、Pb、Mn含量的相对标准偏差均小于1.0%（n=10）.标准加入回收率均在97.0%-101.5%（n=6）范围内.适用于电池锌粉中Mg、Fe、Cu、Pb、Mn的含量控制分析和样品系统分析.     

Direct Multielement Determination of Selected Elements in Rat Urine by Inductively Coupled Plasma Atomic Emission Spectroscopy

Abstract

A method has been developed for the direct determination of dissolved elements in samples of rat urine of less than 2 ml, by Inductively Coupled Plasma Atomic Emission Spectroscopy. The method is capable of measuring copper, iron, magnesium, manganese, phosphorus and zinc.     

Quantifying indium with ion chromatography in hydro‐ and biohydrometallurgical leaching solutions

A methodology has been developed to chromatographically quantify indium in polymetallic (bio)hydrometallurgical processing solutions using the Dionex IonPac CS5A column and pyridine‐2,6‐dicarboxylic acid eluent. Cu(II) and In(III) could be separated by elevating the column temperature to 45°C. The comparatively low stability constant of the In‐eluent complex (log K₂ = 3.8) required typical leaching samples to be diluted in the eluent rather than acid or water to overcome ligand competition between components of the sample solution and the eluent. The methodology was applied to leachates from (bio)hydrometallurgical processing of oxidic flue dust residues and sulfidic zinc ores, where both are promising candidates for the recovery of indium from low grade ores and metallurgical wastes. Indium, ferrous iron, ferric iron, copper, zinc, nickel, and manganese concentrations could be simultaneously quantified. The method was found suitable for samples containing at least 0.25 mg/L indium and an iron to indium ratio of up to 100:1.     

Heavy metal content of a medicinal moss tea for hypertension

The content of various heavy metals (arsenic, cadmium, chromium, copper, iron, lead, mercury, nickel, manganese and zinc) in the moss species Rhodobryum ontariense (Kindb.) Kindb. and its tea are presented in this study. Pursuant to the use of this tea in traditional Chinese medicine for hypertension, the aim of this study was to examine its safety in regard to the metals. All heavy metals were determined by adequate EPA methods. The concentrations of all metals for daily intake in its tea were below the safety levels for human consumption. These results indicate the importance of manganese in R. ontariense tea traditionally used for hypertension and other heart disorders.