卟啉和金属卟啉配合物的合成及其在传感器中的应用

气敏材料是气体（化学）传感器的核心部位,直接影响传感器的稳定性、选择性、灵敏度和响应时间等各种性能。卟啉与金属卟啉配合物具有优良的气敏性能,目前国内外卟啉与金属卟啉传感器已应用于VOCs的检测。该文介绍了卟啉及其结构、合成方法、卟啉和金属卟啉配合物的合成及影响因素;卟啉和金属卟啉在传感器中的应用和对挥发性有机气体的检测原理。     

羊骨基活性炭对溶液中Pb(Ⅱ)的吸附性能

采用本实验室自制的羊骨基活性炭,研究其在不同吸附时间、不同溶液初始浓度、不同投加量、溶液不同的pH值条件下对Pb(Ⅱ)的吸附规律。结果表明:当Pb(Ⅱ)溶液的初始浓度为80mg/L、活性炭投加量为0.10g、吸附时间为6h、溶液温度为45℃时,羊骨基活性炭对Pb(Ⅱ)的去除率高达99%。利用Langmuir吸附等温模型和Freundlich吸附等温模型对其吸附性能的表征得出:羊骨基活性炭对溶液中Pb(Ⅱ)的吸附行为符合Langmuir吸附等温模型和Freundlich吸附等温模型,并且吸附等温曲线在Brunauer五种类型的等温吸附线中比较符合多分子层吸附等温线。     

光波导二氧化氮气敏传感元件的研究

本文用离子交换法制备K+交换玻璃光波导元件,并在其表面固定纳米级敏感层酞菁铜(CuPc)薄膜,利用光波导气体检测系统对NO2气体进行测试.结果表明,该传感元件常温下对NO2等气体有快速、可逆的响应,并具有重现性好,灵敏度高等特点.     

离子—分子反应及其在质谱分析中的应用

利用离子—分子反应 ,不仅可以提供分子离子峰 ,而且可以提高检测的灵敏度 ,了解分子的结构特征。本文根据离子—分子反应的机理 ,介绍了金属离子的亲和力的测定方法和金属离子在化合物上的加合位点 ,并阐述了离子—分子反应在化学电离质谱 ( CI-MS)、碱金属离子化学电离质谱 ( ACI-MS)、电喷雾电离质谱 ( ESI-MS)、快原子轰击质谱 ( FAB-MS)、以及基质辅助激光解吸电离质谱 ( MALDI-MS)中的应用     

新型QTRAP~(TM)四极杆-线性离子阱串联质谱仪的特点及应用

本文介绍新型QTRAPTM 四极杆 -线性离子阱串联质谱仪的基本原理和主要性能 ;并简述在药物筛选及代谢产物分析、蛋白分析和在天然产物结构分析方面的应用     

Direct on-line method to monitor the dynamic structure of noncovalent titanium complexes in solution by using cold-spray ionization time-of-flight mass spectrometry

In this paper, we report the feasibility of using the on-line cold-spray ionization time-of-flight mass spectrometry (CSI-TOFMS) method to monitor directly the labile noncovalent organometallic complexes formed in the substitution reaction between a chiral titanium asymmetric catalyst and organic acid in the toluene solvent. The comparison between the conventional ESI and CSI-TOFMS spectra of [(S)1]2Ti2[(S)2]2 in THF indicated that the CSI-TOFMS is an effective method to characterize the structures of labile organometallic complexes in solution. A new strategy was designed so that [(S)1]2Ti2[(S)2]2 and organic acid solution were delivered independently to the CSI ion source by two infusion syringe pumps, and they mixed at a triple valve, and then the substitution reaction occurred in the sprayer. The mix and reaction time was approximately 5 s and can be adjusted by the length of the PEEK tube and the flow rate. The reaction products were ionized and detected directly by the CSI-TOFMS. Organic acids, such as formic, acetic, phenylpropionic, anisic, and para-methoxylphenylactic acids, were investigated. From the on line CSI-TOFMS spectra, it is observed clearly that one or two (S)2 group(s) can be substituted by the added acid to form new species. The results obtained here demonstrated that the designed strategy with on line CSI-TOFMS is effective and reliable to elucidate the dynamic structure of noncovalent titanium complexes in reaction solution.     

Nafion film/K(+)-exchanged glass optical waveguide sensor for BTX detection

An optical waveguide (OWG) sensor for the detection of BTX gases is reported. The highly sensitive element of this sensor was made by coating the copper Nafion film over a single-mode potassium ion exchanged glass OWG. We used the OWG sensor to detect toluene gas as a typical example BTX gas. The sensor exhibits a linear response to toluene in the range of 0.25-4250 ppm with response and recovery times less than 25 s. The sensor has a short response time, high sensitivity, and good reversibility.     

Simultaneous Structural Identification of Natural Products in Fractions of Crude Extract of the Rare Endangered Plant Anoectochilus roxburghii Using H NMR/RRLC-MS Parallel Dynamic Spectroscopy

Nuclear magnetic resonance/liquid chromatography-mass spectroscopy parallel dynamic spectroscopy (NMR/LC-MS PDS) is a method aimed at the simultaneous structural identification of natural products in complex mixtures. In this study, the method is illustrated with respect to (1)H NMR and rapid resolution liquid chromatography-mass spectroscopy (RRLC-MS) data, acquired from the crude extract of Anoectochilus roxburghii, which was separated into a series of fractions with the concentration of constituent dynamic variation using reversed-phase preparative chromatography. Through fraction ranges and intensity changing profiles in (1)H NMR/RRLC-MS PDS spectrum, (1)H NMR and the extracted ion chromatogram (XIC) signals deriving from the same individual constituent, were correlated due to the signal amplitude co-variation resulting from the concentration variation of constituents in a series of incompletely separated fractions. 1H NMR/RRLC-MS PDS was then successfully used to identify three types of natural products, including eight flavonoids, four organic acids and p-hydroxybenzaldehyde, five of which have not previously been reported in Anoectochilus roxburghii. In addition, two groups of co-eluted compounds were successfully identified. The results prove that this approach should be of benefit in the unequivocal structural determination of a variety of classes of compounds from extremely complex mixtures, such as herbs and biological samples, which will lead to improved efficiency in the identification of new potential lead compounds.     

血浆代谢组同时定性定量分析方法研究

数据非依赖的质谱采集是近年来发展的一种新型多级质谱分析方法，只需一次进样便可同时快速获取所有母离子及其子离子信息。本研究以肺癌血浆样本为研究对象，采用数据非依赖的SWATH（sequential windowed acquisition of all theoretical fragment ions）采集技术，建立了液相色谱-串联质谱法（LC-MS/MS）同时定性定量分析血浆代谢组。基于代谢物数据库识别比对，成功识别了93个代谢物，实现了代谢物的定性分析。对成功识别的代谢物建立定量分析方法并进行方法学考察。结果表明，其中90个代谢物的线性相关系数大于0.99，定量限在1.25~12 000 μg/L之间；其中有86个代谢物可以满足生物样本定量分析的要求，其连续4天的日内精密度和日间精密度均小于20%；在4 ℃下，96 h内的放置稳定性在0.62%~19.35%之间。该方法的覆盖率高，能同时快速准确地对肺癌血浆中癌症相关代谢物进行定性定量分析，也适用于其他生物样品，可以为定量代谢组学分析提供重要的方法学平台。