Arsenic Speciation in Urine and Blood Reference Materials

Acute and chronic exposure to arsenic is a growing problem in the industrialized world. Arsenic is a potent carcinogen and toxin in humans. In the body, arsenic is metabolized to produce several species, including inorganic forms, such as trivalent (As^III) and pentavalent (As^V), and the methylated metabolites such as monomethylarsonic acid, (MMA^V), and dimethylarsinic acid (DMA^V), in addition to arsenobetaine (AsB) which is ingested and excreted from the body in the same form. Each of these species has been reported to possess a specific but different degree of toxicity. Thus, not only is the measurement of total As required, but also quantification of the individual metabolites is necessary to evaluate the toxicity and risk assessment of this element. There are a large number of reference materials that are used to validate methodology for the analysis of As in blood and urine, but they are limited to total As concentrations. In this study, the speciation of five arsenic metabolites is reported in blood and urine from commercial available control materials certified for total arsenic levels. The separation was performed with an anion exchange column using inductively coupled plasma mass spectrometry as a detector. Baseline separation was achieved for As^III, As^V, MMA^V, DMA^V, and AsB, allowing us to quantify all five species. Excellent agreement between the total arsenic levels and the sum of the speciated As levels was obtained.     

熔融反应合成2,2′-联吡啶桥联二（4,4′-联吡啶）类哑铃型化合物

无溶剂反应;联吡啶;固相熔融;哑铃型化合物     

Sensitive trace enrichment of environmental andiandrogen vinclozolin from natural waters and sediment samples using hollow-fiber liquid-phase microextraction

The presence of vinclozolin in the environment as far as the endocrine disruption effects in biota are concerned has raised interest in the environmental fate of this compound. In this respect, the present study attempts to investigate the feasibility of applying a novel quantitative method, liquid-phase microextraction (LPME), so as to determine this environmental andiandrogen in environmental samples such as water and sediment samples. The technique involved the use of a small amount (3 microL) of organic solvent impregnated in a hollow fiber membrane, which was attached to the needle of a conventional GC syringe. The extracted samples were analyzed by gas chromatography coupled with electron-capture detection. Experimental LPME conditions such as extraction solvent, stirring rate, content of NaCl and pH were tested. Once LPME was optimized, the performance of the proposed technique was evaluated for the determination of vinclozolin in different types of natural water samples. The recovery of spiked water samples was from 80 to 99%. The procedure was adequate for quantification of vinclozolin in waters at levels of 0.010 to 50 microg/L (r> 0.994) with a detection limit of 0.001 microg/L (S/N= 3). Natural sediment samples from the Aliakmonas River area (Macedonia, Greece) spiked with the target andiandrogen compound were liquid-liquid extracted and analyzed by the methodology developed in this work. No significant interferences from the samples matrix were noticed, indicating that the reported methodology is an innovative tactic for sample preparation in sediment analysis, with a considerable improvement in the achieved detection limits. The results demonstrated that apart from analyte enrichment, the proposed LPME procedure also serves as clean-up method and could be successfully performed to determine trace amounts of vinclozolin in water and sediment samples.     

EIGHT-POINT STRAIGHT-LINE-NET-DIAGRAMS OF BINARY SIX-PHASE (n+4) MULTISYSTEMS (Ⅱ)——DERIVATION FROM THEORY OF PHYSICALLY REAL NETS

Based on the theory of physically real nets, the 8- point straight-line nets of bi-nary 6- phase (n + 4) multisystems (31 in toto) have been derived directly from the l-point straight-line nets. This result is in complete agreement with that derived fromthe theory of closed nets, indicating the incorrectness of the previous conclusion thatthere is only one 8-point straight-line net which corresponds to only one 8- pointstraight-line-net-diagram for binary 6- phase multisystems.     

高效液相色谱法拆分雷喏嗪

用高效液相色谱法(HPLC)在正相条件下,用自制的涂敷直链淀粉-三(3,5-基苯基氨基甲酸酯)(ADMPC)手性固定相直接拆分了高效低毒的抗心绞痛药物雷喏嗪外消旋体(Ranolazine),并考察了二元及三元流动相体系对样品分离的影响,结果表明,三元流动相中的拆分结果远远好于二元流动相,流动相中不同种类醇改性剂及含量对样品保留时间和立体选择性有不同程度的影响．     

Y2O3, La2O3, Sm2O3对氧化铝瓷烧结及力学性能的影响

研究了3种稀土氧化物对氧化铝陶瓷烧结性能和力学性能的影响.结果表明 含Y2O3,La2O3,Sm2O3的添加剂促进了氧化铝瓷的烧结,提高了氧化铝瓷的力学性能.Y2O3和Sm2O3掺量为0.50%,La2O3掺量为0.75%时氧化铝瓷在1600或1620 ℃保温2 h烧结,相对密度达98.9%以上,强度超过439 MPa,断裂韧性达5.15 MPa·m1/2以上.微观结构分析表明,Y2O3,La2O3,Sm2O3抑止氧化铝晶粒生长,细化晶粒,使晶粒尺寸较均匀形成致密化结构.     

Analysis of the Association Process Between a Series of Phenol Derivatives with Two Novel Fluorinated Stationary Phase Using the Cl− Anion as Retention Marker

Summary Lithium chloride (LiCl) effect on the retention process of a phenol derivative series was investigated on two types of fluorinated stationary phase (i.e. a silica grafted with fluorinated linear alkyl chain (L-FSP) and a silica grafted with fluorinated aromatic ring stationary phase (A-FSP)). The results showed that the solute retention is enhanced when the A-FSP was used instead of the L-FSP due to additional – interactions. For the two fluorinated stationary phases (FSPs), the phenol-FSP association process can be divided into two LiCl concentration domains demonstrated that it was important to take into account the adsorbtion of Cl^– anion on the FSPs. As well, enthalpy-entropy compensation revealed that the solute retention mechanism was independent of the solute molecular structure and confirmed a change on the solute retention mechanism at a critical LiCl concentration value around 0.02M.     

固相萃取-离子色谱-积分脉冲安培法测定人血清中游离氨基酸

比较了磺基水杨酸和无水甲醇沉淀人血清中蛋白质的效果,优化了国产732型阳离子交换树脂进行固相萃取净化的条件和Dionex-600离子色谱分析系统的梯度淋洗条件。用该离子色谱仪检测了谷氨酰胺等14种氨基酸,结果表明,峰面积-浓度的校正曲线的相关系数为0.9900~0.9995,检出限为0.02~0.59mg/L;峰面积的相对标准偏差为1.9%~10.4%;回收率为80.6%~114.8%。     

LaCo13基金属间化合物的磁性能和储氢性能

对LaCo13基金属间化合物在磁致冷材料和储氢材料领域中的应用进行了综述,总结了该系化合物的成相规律、替换元素对相稳定性的影响,讨论了近期的研究进展及存在的问题。作为磁致冷材料应用时,LaCo13基金属间化合物在室温具有巨大磁熵变,而作为储氢合金时该系化合物表现出优异的高温电化学容量。虽然在磁致冷和储氢材料领域尚未对LaCo13基金属间化合物进行实用开发,但作为新型绿色能源材料已经展示出良好的应用前景。     

Clathrate formation and phase transitions in β-hydroquinone

Clathrate thermodynamic stability conditions and the phase transitions associated with either the orientational ordering of the guest molecules or with the condensation of the guest molecules in the host lattice are investigated by means of the common microscopic model. The theory proposed describes the thermodynamic properties of -hydroquinone (Q ) clathrates. The dielectric constant (T) was measured experimentally inQ ·CH₃OH andQ ·SO₂ in the temperature range from 4.2 to 300 K and the phase transitions were found. It is shown that the theory qualitatively explains the experimental data obtained.Dedicated to Professor H. M. Powell.