不分流进样/Cu~(2 )预柱-毛细柱GC/FTIR鉴定环境水中痕量有机污染物

本文介绍一种新的分离分析技术,即不分流进样/Cu~(2 )预柱-毛细柱GC/FTIR,它能彻底消除溶剂影响,实现大容量进样,系统灵敏度比现行GC/FTIR系统高约1～2个数量级。这种技术已成功地用于长江水中痕量有机污染物的分析。     

Impacts of some macromolecules on the characteristics of hydrogels prepared from pineapple peel cellulose using ionic liquid

Composite hydrogels were prepared from pineapple peel cellulose with the combinations of polyethylene glycol (PEG), polyvinyl alcohol (PVA), к-carrageenan (CN), or soluble starch (SH) in 1-allyl-3-methylimidazolium chloride solvent. Impacts of these macromolecules on the texture profile analysis (TPA) parameters, equilibrium swelling ratio (ESR), and sodium salicylate (NaSA) load of the prepared hydrogels were studied. The NaSA release kinetics of the composite hydrogels were also compared. The composite hydrogels exhibited differences in Fourier transform infrared spectroscopy (FTIR), TPA parameters, ESR, NaSA load ratio, and release kinetics. CN addition increased the hardness of the hydrogels, while PEG played an opposite role. SH and PVA could decrease hardness, gumminess, and resilience, and SH could increase the springiness and cohesiveness of the hydrogels. Most of the composite hydrogels exhibited the same basic FTIR features as the simple hydrogel. Freeze-dried composite hydrogels exhibited a markedly higher ESR than the oven-dried ones, and additions of PEG, PVA, CN, and SH showed the same effect. Addition of the PEG and PVA combination could lower the ESR of the hydrogels, whereas additions of the PEG and CN combination or PEG and SH combination could markedly increase the ESR of the hydrogels. Addition of PEG, PVA, CN, and SH respectively could increase the NaSA load ratio of the hydrogels. Oven-drying treatment, additions of the PEG and PVA combination or PEG and CN combination were propitious for extending the NaSA fast-release phase of the hydrogels.     

微孔有机聚合物固相微萃取纤维的制备及在有机氯农药检测中的应用

利用1,3,6,8-四(4-醛基)芘和三聚氰胺为单体合成微孔有机聚合物(MOP),并将其固定在不锈钢丝上,制备成固相微萃取纤维涂层。将其用于顶空固相微萃取(HS-SPME),结合气相色谱-电子捕获检测手段,建立了对大米中有机氯农药的在线检测方法。实验考察了4种实验参数对富集能力的影响,得到了最优的实验条件:萃取温度80℃、萃取时间25 min、NaCl质量浓度200 g/L、解吸时间6 min。在此实验条件下,对有机氯农药的富集倍数达到115~318倍。方法在0.05~50μg/kg范围内具有良好的线性关系,检出限为2.4~11.3 ng/kg。同一纤维及不同纤维富集后测定结果的相对标准偏差范围分别为1.3%~13.1%和2.3%~13.6%。该方法简单、快速,可以实现对实际样品中有机氯农药的痕量分析。     

Inhibitory activity and conformation changes of soybean trypsin inhibitors induced by ultrasound

The inhibitory activities, sulfhydryl bonds and far-UV circular dichroism (CD) spectra of Kunitz and Bowman–Birk soybean trypsin inhibitors (KTI and BBTI) were measured before and after ultrasound treatments. The differences between KTI and BBTI in conformation changes and resistance to ultrasound were observed. The secondary structures of KTI were found to be composed of β-sheet (22.5%), β-turn (16.2%) and random coils (61.4%) while that of BBTI composed of only β-sheet (52.6%) and random coils (47.4%). KTI lost its inhibitory activity more quickly than BBTI, proportionally to the ultrasound amplitudes and sonication durations used. Relevant synchronous phenomena observed included the inactivation of KTI, significant rise in sulfhydryl content and corresponding conformation changes, in which there were dramatic decreases in both β-turn and random coil contents and increase in the β-sheet structure over the entire sonication duration and ultrasonic amplitude scale used by the study. Ultrasound affected the activities and conformations of KTI and BBTI by exerting an influence on their disulfide bonds. For KTI, up to 55% of inhibitory activity could be inactivated, at which about 71.5% of disulfide bonds were altered and the [θ]_200nm value was changed from native −2545 deg cm² dmol⁻¹ to −1827 deg cm² dmol⁻¹. Whereas for BBTI, far-UV CD spectra, β-sheet and random structures were barely affected, only about 5.29% of disulfide bonds were found altered and the [θ]_200nm value was changed only from native −797 deg cm² dmol⁻¹ to −700 deg cm² dmol⁻¹. It is concluded that ultrasound inactivates KTI by inducing a reduction in the disulfide bonds and then changes the conformations.     

高效液相色谱法定量分析人胎肝细胞上清液及细胞裂解液中7-酮基胆固醇

用高效液相色谱法定量分析了７－酮基胆固醇在胎肝细胞上清液及细胞裂解液中的含量。色谱柱为μ－ＰｏｒａｓｉｌＳｉＯ２柱,流动相为正己烷∶异丙醇（９１∶９,Ｖ／Ｖ）。方法回收率高、色谱重复性好、分析速度快。     

16种有机标准物质的研制

介绍16种有机标准物质的研制方法。16种有机标准物质与US EPA、US Supelco及国家标准物质研究中心的同类标准物质比较,均匀性、稳定性及定值准确性均达到或优于其性能指标,符合国家计量技术规范的要求。     

光击穿液体空泡特性的高速图像测量

为了分析激光击穿液体介质过程中的等离子体闪光、空泡脉动、冲击波辐射、空泡溃灭发光等综合效应,将高速摄影技术应用于液体激光击穿研究.采用高功率激光聚焦击穿水、酒精、甘油、硅油等粘性液体,观测到了激光击穿形成的等离子体闪光、空泡脉动及溃灭、空泡溃灭发光及冲击波辐射.通过对激光空泡图像序列的分析,得到了不同液体介质中激光空泡的脉动特征、冲击波辐射等特性.研究结果可为水下激光加工、激光医疗、空化空蚀、能源相关流体力学的研究提供一定的理论和实验支持.     

通过稀土离子和羧酸配体组装成的两种新型的二维配位聚合物的合成、晶体结构及荧光性质

利用水热法合成了两种新型的二维（2D）稀土配位聚合物[Ln(PDC)(OH)(H2O)2]n (Ln = Eu (1) and Tb (2), H2PDC = 3,4-吡啶二羧酸),通过元素分析、红外光谱、热分析和X射线单晶衍射等技术对其进行了表征。单晶结构分析表明这两种配合物都显示出包含有一维Ln-O-Ln链的二维层状结构,层间又进一步通过 π-π 堆积和氢键作用扩展成三维超分子网络结构。此外,这两种配合物的固体在室温下都有强的荧光发射。     

静电纺丝制备图案化无机纳米纤维

静电纺丝技术近几年在制备纳米纤维领域得到了广泛的应用,被认为是批量制备纳米纤维材料最简单有效的方法。本文综述了近几年高压静电纺丝技术制备图案化无机物纳米纤维的纺丝装置和过程,特别详细综述了纺丝过程中纤维直径的变化,利用带电流体动力学(EHD)理论推导出纤维直径变化的运动方程,并对方程进行一定程度的修订,以符合电纺无机物纳米纤维直径的变化;并综述了取向纳米纤维、中空纳米纤维、壳-核结构纳米纤维、纳米线、纳米带、纳米管及多层次结构纳米纤维的构建及其基本性能。最后对电纺制备图案化无机纳米纤维未来发展方向,特别是功能化多层次结构电纺无机纳米纤维制备进行了展望。