化学计量学在分析化学中的应用

从化学定量构效关系、模式识别法、人工神经网络、波谱化学、多元校正分析法等方面对化学计量学在分析化学中的应用进行了综述。阐明了化学计量学在分析化学中的作用及广阔的应用前景。     

小型连续注样电泳芯片及集成化的激光诱导荧光检测系统

通过在芯片进样通道上设计一微孔进样阀,将连续进样系统耦联到芯片上,实现了试样的连续注人.并以小型半导体激光器为光源,借助光纤耦合技术,通过在芯片上设计光纤通道,将自组装的光纤耦合激光诱导荧光检测系统集成到芯片上.还研制了一种小型集成化的连续注样-激光诱导荧光检测电泳芯片分析系统.     

Synthesis, characterization, and biological activities of some transition metal(II) complexes with the thiosemicarbazone derived from 4-[1-(4-methylphenylsulfonyl)-1H-indol-3-yl]but-3-en-2-one

A new 4-[1-(4-methylphenylsulfonyl)-1H-indol-3-yl]but-3-en-2-one thiosemicarbazone (HL) was synthesized derived from 4-[1-(4-methylphenylsulfonyl)-1H-indol-3-yl]but-3-en-2-one. Four transition metal(II) complexes of HL have been prepared. Elemental analysis, molar conductivity, IR, UV, ¹H NMR spectra, and TG-DTA have been used to characterize these complexes. The complexes have the general formula ML₂, where M = Zn, Cu, Co, and Ni. The ligand and its complexes have been studied for their possible biological activity including anti-inflammatory, antibacterial, and antitumour activity in vitro.     

钨硅铁杂多酸盐的Mssbauer谱研究(Ⅱ)——三取代杂多钨硅酸盐异构体

三取代杂多钨硅酸盐SiW_9M_3O_(40)~(n-)有4种异构体,即A-α、A-β、B-α、B-β型。α和β异构体的定向合成条件成熟且性质研究也较深入,故容易鉴别。A和B异构体则不易区分。我们合成了α和β-M_aH_b[SiW_9Fe_3(H_2O)_3O_(37)]·xH_2O(M=K~+,Me_4N~+,Et_4N~++Na~+,Bu_4N~+;a+b=7),测定了四乙基铵钠盐的Mssbauer谱、X射线光电子能谱和磁矩,确定了异构体中Fe的位置以及杂多阴离子的异构类型。     

D-氨基葡萄糖Schiff碱及其金属配合物的抗菌活性

The effects of D-glucosamine schiff base and its metal complexes on the growth of Aerobacter aerogenes were investigated by the microcalorimetry. Among the substances tested. Zn-SG was shown to be the most bacteriostasic, followed by Zn-o-VG and SG (with the Ic50 of 242, 287 and 320 μg•mL-1, respectively). Cu(Ⅱ)-SG showed less inhibitory effect on Aerobacter aerogenes over the concentration rang of 50~300μg•mL-1.     

Application of Short-wave Near-infrared Reflectance Spectroscopy in Controlling Extract of Fructus Cnidii Using Supercritical Carbon Dioxide

Fructus cnidii （Chinese name shechuangzi） is the fruit produced by Cnidium monnieri （L.） Cusson （Umbelliferae）. It is a perennial herb that is used to treat skin-related diseases and gynecopathyell. Recent pharmacological studies have revealed crude extracts or components isolated from fructus cnidii possess antiallergic, antipruritic, antidermatophytic, antibacterial, antifungal, and antiosteoporotic activities. Osthole and imperatorin are the major compounds present in shechuangzi. They are often used as standards for the evaluation of the quality of shechuangzi products.     

液相色谱-串联质谱法测定肉及肉制品中利谷隆及其代谢产物3,4-二氯苯胺残留

建立了液相色谱-串联质谱分析多种肉及肉制品中利谷隆及其代谢产物3,4-二氯苯胺残留的方法。样品用丙酮-乙腈(5:95, v/v)提取,冷冻去脂,经弗罗里硅土固相萃取柱净化后进行液相色谱-串联质谱检测,采用内标法定量。利谷隆及3,4-二氯苯胺在1～500 μg/L范围内呈良好的线性关系,相关系数(r)均大于0.998,方法的定量限(信噪比(S/N)＞10)为10 μg/kg,检出限(S/N＞3)为5 μg/kg。在各种肉及肉制品基质中添加低、中、高3种不同水平的利谷隆及3,4-二氯苯胺,其回收率范围分别为88.3%～101.2%和91.6%～101.6%,相对标准偏差(RSD)分别为4.8%～13.7%和4.7%～11.8%。结果表明所建立的方法可以满足肉及肉制品中利谷隆和3,4-二氯苯胺残留量的检测需要。     

基于2-硫代海因的氟离子探针

通过异亮氨酸甲酯盐酸盐与4-硝基苯基异硫氰酸酯或4-氰基苯基异硫氰酸酯反应合成2-硫代海因探针1和2.在N,N-二甲基甲酰胺(DMF)中,用系列含阴离子的四正丁基铵盐来评价其阴离子识别能力.加入F-后,1和2的DMF溶液由无色立即变为黄色,而加入Cl-,4HSO-,Br-,3NO-和3 2CH CO-均不变,表明1和2对氟离子显示出良好的识别性能.核磁滴定氢谱揭示了F-与2-硫代海因的氢键作用引发了1和2的识别,结合常数显示1比2对F-更敏感.此外,1作为化学传感器还可以制成试纸检测F-.     

Urea-based polyacetylenes as an optical sensor for fluoride ions

Novel acetylenes carrying urea groups, 1-(4-ethynylphenyl)-3-(4-nitrophenyl) urea (1), 1-(4-propargyl)-3-(4-nitrophenyl) urea (2), were synthesized and polymerized with rhodium catalyst. Polymers [poly(1) and poly(2)] with moderate molecular weights were obtained in good yields. The anion sensing ability of poly(1) and poly(2) was estimated using the tetra-n-butylammonium (TBA) salts of a series of anions in DMF. Upon the addition of F-, the color of the DMF solution of poly(1) and poly(2) immediately turned to a different color, while the color of solution changed slightly upon addition of Cl-, HSO4-, Br-, and NO3-, indicating the F- sensing ability of poly(1) and poly(2). The 1H-NMR titrations of poly(1) revealed that the colorimetric response of poly(1) was triggered by the urea/F- interaction through the hydrogen bonding and/or deprotonation process. The absorption spectra titration and Hill plot analysis were carried out to measure the F- binding ability, and the Hill coefficient in the poly(1)/F- complexation was found to be 5.8. This result clearly indicated that this binding mode between poly(1) and F- was based on a positive homotropic allosterism.