Improved method for analyzing estrogens in water by liquid chromatography-electrospray mass spectrometry

An improved LC-electrospray ionization MS method was established for four estrogens (17beta-estradiol (E2), estriol (E3), estrone (E1), and ethynyl estradiol (EE)) in environmental water. Almost complete separation of all estrogens was achieved on a phenyl column with methanol/water as the mobile phase. Quantification was achieved in the negative ionization mode using selected ion monitoring. The instrumental detection limits were 20-30 ng/l for the four analytes. In Milli-Q spiked water, the recoveries of the four estrogens were 72-81%, which was similar to those found for river water spiked with the corresponding deuterated estrogens. The detection limits for the four estrogens in river water were 0.1-0.2 ng/l. The method was used to detect residual estrogens in the Tonghui River, which receives water from a municipal sewage treatment plant in Beijing; E1 (1.1 ng/l) and E2 (0.2 ng/l) were detected.     

Detection of Anti-Ulcer Drugs and Their Metabolites in Horse Urine by Liquid Chromatography – Mass Spectrometry

This paper describes a convenient method for the extraction and detection of eight anti-ulcer drugs simultaneously in horse urine, a relatively complex and viscous matrix, using a single-step liquid-liquid extraction followed by high-performance liquid chromatography – mass spectrometry (LC-MS). Anti-ulcer drugs were isolated from horse urine by salting out and liquid-liquid extraction. Detection of these drugs at concentrations below 1 ng mL^?1 could be achieved using LC-MS-MS in the positive atmospheric pressure chemical ionisation (APCI) mode. The above analysis was also extended to elimination studies of horses administered with ranitidine and omeprazole. The urinary elimination data of these two drugs suggest that ranitidine was eliminated from horse urine at a much slower rate than omeprazole. In addition, three ranitidine metabolites and six omeprazole metabolites were identified for the first time in equine urine samples.     

Pt对Mo基催化剂还原-硫化过程的影响

采用脉冲硫化、连续硫化、程序升温还原、程序升温及程序降温电导及X射线衍射等方法研究了贵金属Pt对MoO3催化剂还原-流化过程的影响及Pt对MOS2配位不饱和活性中心形成的影响．结果表明，Pt担载或在MoO3上可以促进MoO3的还原-硫化，使MoO3的还原-硫化温度大大降低Pt担载在MoSw上可促进MoS2的部分还原形成配位不饱和的钼中心     

铜离子交换改性的沸石催化剂上甲烷的非氧芳构化

已有研究表明，ＭｏＯ３／ＨＺＳＭ５是甲烷非氧芳构化的优良催化剂，在９７３Ｋ下甲烷转化率达６％～８％，苯选择性高于８０％，这为非氧气氛下甲烷的芳构化反应展示了非常诱人的前景［１～１２］．但是，该催化剂的活性和稳定性尚有待进一步提高，目前已有使用Ｐｔ，...     

基于磁泳的生物分离分析技术

利用磁场诱导的微粒运动即磁泳对磁响应性粒子进行精细分离,是近年来发展起来的选择性分离细胞和高分子量核酸的有效技术。本文在阐明磁泳分离原理的基础上,介绍了磁泳分离的分流薄层分级技术、四极磁场流动分离技术和微芯片上的自由流磁泳分离技术的装置构造、工作原理及其在生物分离分析中的应用。     

Structure of thiocyanate adlayers on Rh(111): an in situ STM study

In situ scanning tunneling microscopy (STM) was used to examine the structure of thiocyanate adlayers specifically adsorbed on Rh(111) in solutions of potassium hydroxide and perchloric acid, both containing potassium thiocyanate (KSCN). An atomically flat terrace-step structure was consistently observed on Rh(111) surfaces prepared by the flame-annealing-quenching method. The Rh(111)-(1 × 1) atomic structure was discerned on the atomically flat terrace even in the alkaline solution. High-resolution STM images disclosed two different structures of the SCN⁻ adlayers, () and (2 × 2), in the alkaline and the acidic media, respectively. In each structure, an individual adsorbed SCN⁻ ion appeared as a single spot with a constant corrugation height in STM images, suggesting that SCN⁻ ions adsorbed predominantly with their S-ends at particular bonding sites on Rh(111). The difference in the adlayer structure in the two solutions can be attributed to the interaction between adsorbed SCN⁻ and coadsorbed K⁺ in the alkaline solution, and is different from that between adsorbed SCN⁻ and H⁺ in the acidic solution. Received: 26 February 1997 / Accepted: 3 March 1997     

Molar conductivity calculation of Li-ion battery electrolyte based on mode coupling theory

A method is proposed to calculate molar conductivity based on mode coupling theory in which the ion transference number is introduced into the theory. The molar conductivities of LiPF6, LiClO4, LiBF4, LiAsF6 in PC (propylene carbonate) are calculated based on this method. The results fit well to the literature data. This presents a potential way to calculate the conductivities of Li-ion battery electrolytes.     

丙酮肟与某些芳烃相互作用的~1H核磁共振研究

Hatton和Richards通过对酰胺分子的~1H NMR谱溶剂效应的研究,提出了DMF与苯生成分子络合物的模型.如果络合物按1:1生成,那么将出现一个“饱和点”,在这点上甲基的芳香溶剂诱导位移(ASIS)的变化趋势或程度将出现一个明显的变化,事实上随着苯的摩尔分数从0到1逐渐增加时,化学位移总是有规则的逐渐移向高场.这就显示了分子络合物观点的局限性.它能被一些研究者所支持和接受,是因为它能够解释两个甲基共振峰先重合而后又分离的现象.     

新材料的发展与分析化学

文章介绍了新材料的重要性及发展方向,分析化学在新材料研制中起着耳目的作用,另一方面新材料也为分析化学的进展提供了课题与条件。微量分析、微区分析、表面分析是此领域中的重点。在未来的发展中,分析化学在材料的发展中的地位不会改变,并期待着分析灵敏度与空间分辩率的进一步提高。     

丙烯选择氧化铋钼铁复氧化物催化剂组成,结构及性能的研究

采用XRD、Raman、XPS及催化剂性能评价等手段,考察了Bi_3(FeO_4)(MoO_4)_2和Fe_2(MoO_4)_3分别存在及两者共存时对Bi-Mo复氧化物体系催化性能的影响.结果表明,这两种含Fe物种的存在都有助于改善Bi-Mo系复氧化物催化剂对丙烯选择氧化反应的催化性能.但两者在作用机理上有所不同.Fe_2(MoO_4)_3本身无催化活性,但在反应条件下可部分还原为FeMoO_4形成Fe~(3+)/Fe~(2+)氧化还原对;且其地结构上与α-Bi_2(MoO_4)_3相匹配,这些因素都有助于促进催化体系中电子和氧物种的传递及催化剂表面活性中心的再生,从而提高催化性能.Bi_3(FeO_4)(MoO_4)_2在反应条件下也可形成Fe~(3+)/Fe~(2+)氧化还原对,但由于其Fe~(3-)所处的化学环境与Fe_2(MoO_4)_3很不相同,且Fe的含量也不及Fe_2(MoO_4)_3,因此它在促进催化体系中电子和氧物种的传递及催化剂表面活性中心的再生等方面的性能较差,但它对提高催化剂表面的活性中心(Bi-Mo对)数目有贡献.