秦岭德昌香薷不同提取方法挥发油成分分析

采用分析型超临界CO2流体萃取技术(SFE-CO2)与传统水蒸汽蒸馏法(SD)分别提取德昌香薷挥发油,并通过气相色谱-质谱联用技术测定了提取物的化学成分.从中分别鉴定出35个和50个化合物.结果显示:白苏酮、香芹酚、α-石竹烯、石竹烯、柠檬醛、芳樟醇、对薄荷烯醇等是德昌香薷挥发油的主要成分.对比两种不同方法的分析结果可知,超临界萃取法比传统水蒸气蒸馏法能得到更多的极性组分,因而其被广泛应用于中草药的分析.     

硅藻土TBP反相萃取层析法连续分离钼和锗

研究了以6mol/L盐酸做流动相，以负载有磷酸三丁酯（TBP）的硅烷化白色担体做固定相，反相萃取层析法连续分离Ge和Mo与其它干扰高子如W、Sb、Fe等的分离条件。方法可将Ge、Mo与W、Sb、Fe、Sn等完全分离，并已应用于中草药中微量锗和钼的分离。     

Use of a keeper to enhance the recovery of volatile polycyclic aromatic hydrocarbons in HPLC analysis

Summary The recorveries of volatile polycyclic aromatic hydrocarbons in HPLC analysis may be enhanced if a long-chain alcohol, e.g. 1-hexanol or 1-octanol, is used as keeper in the solvent-evaporation step. Even under the harsh conditions of the vacuum-concentrator centrifuge, recoveries of more than 90% were achieved for 14 of the 15 PAH tested. The use of liquid-liquid extraction (LLE) eliminates the problem of adsorption of highly condensed aromatics by the wall of the sampling bottle. The combination of LLE with vacuum-controlled rotary evaporation and use of a keeper yielded overall recoveries between 50 and 130%, for most substances close to 100%, from tap water spiked with trace concentrations. Presented at the 21^st ISC held in Stuttgart, Germany, 15^th–20^th September, 1996     

光度法研究聚乙二醇-硫酸铵-邻苯三酚红体系中铋(Ⅲ), 铁(Ⅲ), 铜(Ⅱ), 镍(Ⅱ), 钴(Ⅱ), 铅(Ⅱ)的萃取分离

本文研究了在聚乙二醇(PEG)-硫酸铵[(NH_4)_2SO_4]-邻苯三酚红(PR)体系中Bi(Ⅲ),Fe(Ⅲ),Cu(Ⅱ),Ni(Ⅱ),Co(Ⅱ),Pb(Ⅱ)的萃取行为。实验结果表明,Bi(Ⅲ)在pH3.5～6.5及Fe(Ⅲ)在pH4.0～7.0范围内可以被PEG相几乎完全萃取,而Cu(Ⅱ),Co(Ⅱ)在pH1.0～7.0,Pb(Ⅱ)在pH2.0～7.0,Ni(Ⅱ)在pH1.0～4.5则不被萃取。从而实现了将Bi(Ⅲ)(pH3.5),Fe(Ⅲ)(pH5.0)与Cu(Ⅱ),Co(Ⅱ),Pb(Ⅱ),Ni(Ⅱ)混合离子的定量分离。同时探讨了PEG相的萃取机理。     

Solubility and polarity parameters for pyridinecarboxamides and their complexes with copper(II) as determined by inverse gas chromatography

Pyridinecarboxamides and their complexes with copper(II) were characterized by means of inverse gas chromatography. The investigated amides were extractants of copper(II) from solutions with a high chloride concentration. Solubility and polarity parameters were used to quantitate the properties of the extractants. The influence of the extractant's structure upon its properties are presented and discussed as well as the dependence of the physicochemical parameters on the introduction of the metal ion into the molecular structure.     

HIRFL-CSR主环慢引出设计

对HIRFL-CSR工程的主环（CSRm）的共振慢引出进行了设计，并采用Winagile程序对引出过程进行了初步的计算机模拟。主环慢引出采用幅度和动量选择引出机制，其引出通道和快引出通道相同。采用了1/3整数共振慢引出机制来获得约1 s的较均匀的引出束流，该引出束流的水平发射度小于1 πmm·mrad。     

聚乙二醇-硫酸钠-萃取剂体系中萃取剂及金属离子光谱性能

本文用光度分析法,研究了在聚乙二醇-硫酸钠-萃取剂双水相体系中茜素S、孔雀绿和PAR的萃取行为,提出了萃取剂与聚乙二醇之间水作为中介的氢键作用。探讨了Zr(Ⅳ),Ti(Ⅳ),La(Ⅲ)几种稀有金属离子在聚乙二醇-硫酸钠-茜素S体系中萃取条件,结果表明,在pH 1-3缓冲溶液中,Zr(Ⅳ)几乎完全可被PEG相萃取,La(Ⅲ)离子部分被萃取,而Ti(Ⅳ)离子则不被萃取,通过控制溶液酸度(pH2),实现了Ti(Ⅳ)与Zr(Ⅳ)的萃取分离。     

中草药中微量锗和钼的同时测定

本文采用硅藻土 TBP反相萃取层析 分光光度法同时测定了中草药中的锗和钼的含量 ,获得了锗、钼含量较高的中草药。中草药样品经处理、消化后 ,用盐酸将试样中HCl浓度调至 6mol·L-1,加入以负载有磷酸三丁酯 (TBP)的烷基化硅藻土做固定相的层析柱。用 4mol·L-1盐酸以 0 5mL·min-1的流速洗脱锗 ,苯基荧光酮 CTMAB分光光度法测定锗 ,Ge PF CTMAB络合物的λmax=5 10nm ,摩尔吸收系数ε510 =1 6 7× 10 -5L·mol-1·cm-1。用 0 5mol·L-1盐酸以 0 5mL·min-1的流速洗脱钼 ,苯基荧光酮 CTMAB分光光度法测定钼 ,Mo PF CTMAB络合物的λmax=5 2 5nm ,摩尔吸光系数ε52 5=1 16× 10 -5L·mol-1·cm-1。该方法可对样品中的锗和钼同时测定 ,简便易行 ,具有较高的灵敏度 ,而且能有效地避免共存离子的干扰。     

3D simulation of InGaN/GaN micro-ring light-emitting diodes

We employed the APSYS software to perform 3D electrical and ray-tracing simulations on micro-ring light-emitting diodes (LEDs) to verify previous experimental findings that they have higher extraction efficiency than micro-disk and broad area LEDs. 3D ray-tracing indicates the importance of inter-ring optical interactions. Furthermore we found that the higher light extraction efficiency is at the expense of reduced internal quantum efficiency (IQE) as injection current is increased.     

示差折光检测-固相萃取和高效液相色谱法测定水果中的糖

研究了高效液相色谱法测定水果中的糖。水果样品的糖提取液用 Waters Sep- Pak- C18固相萃取小柱预分离 ,以 Waters Sugar- Pak- 1钙型阳离子交换柱为固定相 ,0 .0 5 g· L-1EDTA钙钠水溶液为流动相分离 ,示差折光仪为检测器检测。蔗糖、葡萄糖和果糖的检出限分别为 2 mg/ L、4 mg/ L和 4 mg/ L,RSD在0 .76 %— 1.8%之间 ,标准回收率在 97%— 10 3%之间。本方法用于几种水果样品的测定 ,结果令人满意。