凝胶渗透色谱-气相色谱-离子阱质谱法测定桔梗原药和当归提取物中101种农药残留

建立了凝胶渗透色谱（GPC）-气相色谱-离子阱质谱同时检测桔梗原药和当归提取物中101种农药残留的分析方法。方法采用乙腈超声辅助提取桔梗原药和当归提取物,浓缩提取液至近干后用乙酸乙酯-环己烷（1∶1, v/v）复溶,采用凝胶渗透色谱法（选取40 cm长、内径20 mm的凝胶渗透色谱柱）对样品进行净化,弃去前段含脂类、色素等杂质的流出液,收集17~30 min洗脱液并旋转蒸发浓缩至近干,甲苯1 mL定容上机。选用DB-5MS毛细管色谱柱分离待测物,通过离子阱质谱实现对101种农药残留的高效检测。方法通过优化前处理条件和离子阱二级质谱参数,有效降低了复杂中药基质对待测化合物的干扰,最大限度提高了样品中农药的定量准确性和回收率,101种农药3水平添加的平均回收率为58.3%~108.9%,每个添加水平10次独立重复测定的相对标准偏差为0.4%~16.5%,检出限（LOD）范围为0.2~40.0 μg/kg,可满足当前韩国、日本、欧洲规定的最大残留限量（maximum residue limits, MRLs）要求。方法具有操作简单快速、灵敏度高、重复性好等特点,凝胶渗透色谱技术的应用克服了固相萃取小柱净化容量不足的弊端,离子阱技术的应用可以进一步排除共流出基体杂质的干扰,提高定量和定性的准确性,检测效果优于常用的气相色谱-质谱法,是对中药中同时分析多种农药残留检测方法的有益补充。     

过渡金属原子X (X=Mn、Fe、Co)掺杂单层Janus WSSe的第一性原理研究

二维Janus WSSe作为一种新兴的过渡金属硫族化合物(TMDs)材料,由于其打破了面外镜像对称性,且具有内在垂直压电和强Rashba自旋轨道耦合效应等丰富的物理特性,在自旋电子器件中具有巨大的应用潜力。本文基于密度泛函理论的第一性原理平面波赝势方法计算了过渡金属原子X(X=Mn、Fe、Co)掺杂单层Janus WSSe的电子结构、磁性和光学性质。结果表明：在Chalcogen-rich(硫族元素为多数元素)条件下的掺杂比在W-rich(钨元素为多数元素)条件下的掺杂展现出更高的稳定性,且掺杂后所有体系均表现出磁性。值得一提的是,对该体系进行Mn掺杂后,自旋向上通道出现杂质能级,WSSe由原来的非磁性半导体转变成磁矩为1.043μ_B的铁磁性半金属。而Fe、Co的掺杂使得自旋向上通道和自旋向下通道均出现杂质能级,呈现出磁矩分别为1.584μ_B、2.739μ_B的金属性。此外,掺杂体系的静态介电常数都显著增加,极化程度增强,且介电函数虚部和光吸收峰都发生了红移,说明掺杂有利于对可见光的吸收。     

Transpiration-inspired Capillary for Synchronous Synthesis and Patterning of Silver Nanoparticles

Traditional synthesis strategy of nanomaterials with complicated process and high cost limits their applications. Here, we propose a facile process for the synchronous synthesis and patterning of silver nanoparticles(Ag NPs) through the self-driven microchannel reactor with the capillary effect inspired by transpiration. The evaporation contributes to capillary and accumulation effects in the microchannels. The silver reactant-containing droplets can be spontaneously divided and distributed in multiple microchannels during the whole fabrication process by the capillary effect. The newly formed Ag NPs at the gas-liquid interface can be assembled on both sides of the microchannels by the accumulation effect. The capillary effect decreases the disturbances, which ensures the uniformity of the patterning. By the combination of microchannels with different widths, various Ag NPs-assembled patterns with stable electrical properties are achieved. This efficient strategy with a simple fabrication procedure is towards the technological engineering of nanoscale architected materials.     

滴定分析的终点误差随待测物浓度及反应平衡常数单调变化之商榷

为了获得滴定分析的终点误差随待测物浓度、反应平衡常数这两个因素变化的准确规律,推导了有别于林邦终点误差公式的终点误差计算式,根据该式可以判断每个因素对计算结果的影响,结合在配位滴定分析和酸碱滴定分析的具体应用,结果发现：这两个因素其大小的变化不会一定导致终点误差绝对值的单调变化。     

MOLECULAR DESIGN SYNTHESIS AND PROPERTIES OF SIX KINDS OF MULTIPHASE (STYRENE-ETHYLENE OXIDE)COPOLYMERS

Multiphase copolymers of styrene (S) and ethylene oxide (EO) are amphiphilic, because of the hydrophobic and amorphous polystyrene (PS) segments and the hydrophilic and crystalline polyoxyethylene (PEO). They have many uses including polymeric surfactants, electrostatic charge reducers, compatibilizer in polymer     

STUDY ON THE CONFORMATIONAL PROPERTIES OF RIGID POLYELECTROLYTE SPU IN SOLUTION

The conformation and dimension of SPU polyanion have been studied by viscosity and quasi-elastic light scattering methods. The rigidity of SPU is somewhat similar to CMC and its hydrodynamic radius decreases only slowly with increasing concentration of NaCl.     

CLIMATIC CHANGE SINCE LITTLE ICE AGE RECORDED BY DUNDE ICE CAP

The climatic change since the Little Ice Age recorded in the Dunde Ice Cap is presentedin this paper. There have been three cold periods and three warm periods since 1400AD.Among them, the coldest one was in the 17th century. Many evidences verified the three coldand warm variations recorded in the Dundc Ice Cap. But it was found from the comparison between the Dunde Icc Cap climatic record and thewinter temperature record in Shanghai that there was a temporal dfference in climatic changebetween East China and West China. The general trend is that the cooling and warmingprocesses in West China were earlier than that in East China. In the Dunde Ice Cap, it isnow in an anomalous warm period, while it is not as warm as in Dunde Ice Cap recordaccording to the winter temperature in Shanghai. In addition to the possible cause of temporaldifference in climatic change between West China and East China, another possible cause isthat the greenhouse effect of CO_2 may already be recognizable in the Dunde Ice Cap a     

CYTOLOGIC AND EMBRYOLOGIC STUDIES ON APOMICTS DISCOVERED FROM MALE STERILITY LINE C1001 IN RICE (Oryza sativa L.)

Cytologic and embryologic studies on the reproductive pattern of male sterility line C1001 in rice (Oryza saliva L.) indicated that several types of apomixis were discovered in partial strains of male sterility line C1001 in rice. Under a fully separate condition, two possible apomixis embryogenesis ways in the ovules were observed: One way was that the embryo was initiated from the somatic cells of the ovules, and then pushed against the embryo sac to develop into a mature embryo. The other way was that the embryo was from the unfertilized egg cell or one of synergids, and then developed into a mature embryo in the form of haploid parthenogenesis without forming endosperm. Besides, the antipodal cells migrated in the embryo sac, and their cytoplasm became thin and vacuolated while mitosis was taking place, giving rise to a multicellular structure or a group of large cells each containing several nuclei. This paper also discusses the significance and patterns of apomixis in rice C1001.     

SYNTHESES OF THE SOLUBLE,HIGH MOLECULAR WEIGHT AND LADDERLIKE POLYPH ENYLSILSESQUIOXAN E AND COPOLYMETHYLPHENYLSILSESQUIOXANES BY PREAMMINOLYSIS METHOD

Soluble, high molecular weight (MW) and ladderlike polyphenylsilsesquioxane (LPPSQ) and its copolymers, ladderlike random and block copolymethyiphenylsilsesquioxanes(LR-PMPSQ and LB-PMPSQ)have been prepared by preamminolysis, hydrolysis and polycondensation reactions. The preparation method can be carried out easily at the temperature below 95℃with high yield of 95 %, instead of the conventional way by using high-boiling solvent and any reaction activator or by precipitation with methanol. Three kinds of ladderlike polymers have been characterized. The MW's of the polymers reached to 10~6 without noticeable gelling. The scheme for synthetic route has been proposed.     

三环己基锡芳氧乙酸盐的合成及其结构表征

三环己基锡衍生物(Cy_3SnX,Cy=环己基,X=配体或取代基)是一类具有较强生物活性的有机锡化合物,它们广泛用作杀螨剂,杀菌剂和海洋防污剂。有关三环己基锡芳氧乙酸盐的合成至今报道很少。Bubblitz 合成了两个三环已基锡芳氧乙酸盐,此后,Matsuda 等人制备了三环已基锡-2,4-二氯苯氧乙酸盐,它们都具有良好的杀螨、杀菌活性,后者还可应用于海洋