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101.
As interfered with by alkali and alkaline earth metal halides added as the matrix in an acetylene/air flame, the fluorescence quantum yield of In as the analyte in a laser‐induced fluorescence (LIF) flame spectrometry has been thoroughly characterized. The fluorescence quantum yield is determined by a ratio of F to A, where F is the measured fluorescence of In and A is the difference between the absorption signals recorded for the analyte and the blank solutions. The normalized fluorescence signal is treated to prevent deviations due to variations of the atomization efficiency under the conditions with and without the matrix added. The fluorescence quantum yield is measured to be almost independent of the matrix concentration up to 500 ppm (μg/mL) studied, under conditions of either optical unsaturation or saturation. By considering a quenching effect induced by electron‐atom collisions, the calculated fluorescence quantum yields are consistent with our observations. 相似文献
102.
On-line sample-pre-treatment schemes for trace-level determinations of metals by coupling flow injection or sequential injection with ICP-MS 总被引:1,自引:0,他引:1
Within the last decade, the first generation of flow injection (FI) has been supplemented by sequential injection (SI), also termed the second generation, and, recently, by the third generation, i.e., SI-Lab-on-Valve (SI-LOV). As apparent from the literature, FI and/or SI have become dominant as substitutes for labor-intensive, manual, sample-pre-treatment and/or solution-handling procedures prior to analyte detection by inductively coupled plasma mass spectrometry (ICP-MS). The present review presents and discusses the progress of the state of the art in implementing miniaturized FI/SI systems for on-line matrix separation and pre-concentration of trace levels of metals with detection by ICP-MS. It highlights some of the frequently applied on-line, sample-pre-treatment schemes, including solid phase extraction (SPE), on-wall molecular sorption and precipitate/(co)-precipitate retention using a polytetrafluoroethylene (PTFE) knotted reactor (KR), solvent extraction-back extraction and hydride/vapor generation. It also addresses a novel, robust approach, whereby the protocol of SI-LOV-bead injection (BI) on-line separation and pre-concentration of ultra-trace levels of metals by a renewable microcolumn is interfaced to ICP-MS, as conducted in the present authors' group. It discusses the future outlook in this field. 相似文献
103.
选取铝、铜、镁、钙、铁、锰和锌等7种元素的9条谱线,研究电感耦合等离子体原子发射光谱法对其测定时易电离元素钾、钠的基体干扰。结果表明:易电离元素对待测元素具有较明显的干扰作用,而增大射频发射功率及降低雾化器压力可有效地抑制易电离元素对待测元素的干扰。 相似文献
104.
MALDI质谱检测蛋白质与富勒醇的非共价复合物 总被引:4,自引:0,他引:4
基质辅助激光解吸电离(MALDI)质谱由于受到酸性基质、样品制备、激光诱导聚合和基质加合物的形成等条件的限制而难以用于非共价复合物的检测.本文以芥子酸为基质,观察到蛋白质与富勒醇的特殊相互作用,一些质谱特征,如质量数迁移、宽的加合峰和定量结合比表明,在蛋白质和富勒醇之间形成了特殊的非共价复合物.其中,血红蛋白与富勒醇的结合比是1:4,而肌红蛋白与富勒醇的结合比是1:1.实验结果表明:富勒醇可用来保护血红蛋白,有在酸性介质中防止其分解的作用.因此,通过在基质组份中添加特性有机化合物保护被测样品,有可能实现用MALDI质谱测定四级结构蛋白质的分子量. 相似文献
105.
聚合物共混物脆韧转变性能研究 Ⅲ.分散相形态参数之间的关系 总被引:4,自引:2,他引:4
为了研究形态(特别是分散状态)对聚合物共混物韧性的影响,建立了准网络形态模型,定义了分散相分布系数(ξ,0<ξ1),并给出其物理意义,推导了基体层厚度的计算公式,研究了形态参数的变化对基体层厚度的影响.对于常见的无规形态,ξ≈1.对于准网络形态,ξ<1,并且不是常数.计算结果表明,减小ξ和分散相粒径及其分布、增大其体积分数有利于减小基体层厚度.从理论上证明了准网络形态比无规形态更有利于减小基体层厚度. 相似文献
106.
107.
In this paper, we propose the construction of merging arrangements for combining the information from various runs as a powerful approach to improve the resolution. The bacteriorhodopsin (bR) photocycle has been chosen in this study as an example dealing with the protein dynamics monitored by means of time-resolved step-scan FT-IR spectroscopy. The possibilities of matrix merging are evaluated and results are compared with those from the analysis of individual and augmented matrices. As a conclusion, this strategy provides excellent results for the analysis of this type of time-resolved FT-IR data. 相似文献
108.
The total synthesis of trifluoromethyl (Tfm) analogs of known nanomolar matrix metalloproteinases (MMPs) inhibitors has been performed. The synthetic protocol is based on a moderately stereoselective aldol reaction of trifluoropyruvate with an N-acyl-oxazolidin-2-thione for the construction of the core α-Tfm-malic unit. Both the diastereomeric forms of the target α-Tfm-malic hydroxamates showed micromolar inhibitory potency toward MMP-2 and 9, with a substantial drop with respect to the parent unfluorinated compounds. 相似文献
109.
In the present study, humic acids (HAs) were applied as both a matrix for matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) and an adsorbent of magnetic solid phase extraction (MSPE) for the first time. As natural macromolecule compounds, HAs are inherently highly functionalized and contain laser energy absorbing–transferring aromatic structures. This special molecular structure made HAs a good candidate for use as a MALDI matrix in small molecule analysis. At the same time, due to its good adsorption ability, HAs was prepared as MSPE adsorbent via a simple co-mixing method, in which the commercially available HAs were directly mixed with Fe3O4 magnetic nanoparticles (MNPs) in a mortar and grinded evenly and completely. In this process, MNPs were physically wrapped and adhered to tiny HAs leading to the formation of magnetic HAs (MHAs). To verify the bi-function of the MHAs, Rhodamine B (RdB) was chosen as model compound. Our results show that the combination of MHAs-based MSPE and MALDI-TOF-MS can provide a rapid and sensitive method for the determination of RdB in chili oil. The whole analytical procedure could be completed within 30 min for simultaneous determination of more than 20 samples, and the limit of quantitation for RdB was found to be 0.02 μg/g. The recoveries in chili oil were in the range 73.8–81.5% with the RSDs less than 21.3% (intraday) and 20.3% (interday). The proposed strategy has potential applications for high-throughput analysis of small molecules in complex samples. 相似文献
110.
血清中甲胎蛋白(AFP)的准确测量对于癌症的临床诊断和治疗具有重要意义.电感耦合等离子体质谱法(ICP-MS)具有灵敏度高、检出限低、多元素同时检测等优点,但用于血清中低丰度蛋白的检测时,检出限常不及荧光检测法,因此,提高ICP-MS免疫分析测量低丰度蛋白质时的灵敏度具有重要意义.本研究发现,增强液能很大程度增加Eu信号强度,选取醋酸、醇类、EDTA三类有机试剂模拟增强液来探索增强机理.结果表明:酸性体系能增加目标元素在基体中的稳定性,减少其在管壁的吸附;碳原子或分子容易接受电子提高Eu的电离效率;EDTA能与金属离子结合,减少吸附,但同时EDTA与其它金属结合引入更多的干扰,从而使空白信号增大,5% HAc既能满足酸性要求也能满足含碳量要求,作为基体时铕的灵敏度最高,同时也不影响空白信号.因此选择5% HAc作为解离液,并应用于人血清中甲胎蛋白含量的测定,线性范围为1~600 μg/L,检出限为0.57 μg/L,采用基体改进ICP-MS测量人血清中AFP的含量与TRFIA测量结果一致,且精密度要优于TRFIA的测量结果. 相似文献