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91.
92.
93.
一阶导数停流法测定药物和饮用水中的铁 总被引:3,自引:0,他引:3
本文利用Fe^3+离子催化H2O2氧化四甲基对苯二胺的反应,将采用停流技术获得的动力学曲线转换成一阶导数曲线,根据导数峰高值与Fe^3+离子浓度的线性关系测定药物和自来水中的含量,本方法的线性范围为4.0-40.0ngFe^3+/ml,相对标准偏差小于2.5%,标准加入回收率在98.7%-101%之间,检测限为1.92ngFe^3+/ml。对照实验结果表明,导数动力学法比一般非导数动力学法具有线关 相似文献
94.
Krzysztof Maruszewski Marek Jasiorski Witold Wacławek Wiesław Stręk Marek Lisowski 《Journal of Sol-Gel Science and Technology》1998,13(1-3):585-586
A series of silicate xerogels with entrapped chiral amino acids have been obtained via sol-gel technology. The transparent, glassy samples obtained exhibit chirality in the bulk due to the presence of the entrapped asymmetric molecules. Measurements of the optical activity of the doped xerogel samples revealed that the entrapment did not significantly influence the optical activity observed for liquid solutions of the amino acids. Thus, the sol-gel method enables the preparation of amorphous optical materials exhibiting properties of strictly spatially defined molecular systems. Apart from the obvious optical applications, such porous materials with asymmetric centers might find interesting applications in chiral chemical syntheses and separations. 相似文献
95.
Underpotential deposition studies of copper on glassy carbon 总被引:1,自引:0,他引:1
Studies on the deposition and dissolution of copper from 0·5 M sulphuric acid solutions onto glassy carbon (GC) using potential
sweep techniques indicated that an additional peak occurs at higher positive potentials than the bulk stripping peak. This
peak is identified as due to the stripping of underpotential deposited (UPD) copper. Results of investigations on the effect
of sweep rate, deposition potential and time of deposition on the peak characteristics of UPD and bulk deposited copper are
also reported. 相似文献
96.
Four new stationary phases for HPLC were prepared by modifying silica gel with a trifrnctional aminoalkyl silane. A conjugated π-electron system was linked to the amino group either directly or with a carboxylic anhydride as a spacer in between. Characterization and dynamic measurements of the new stationary phases were performed by solid state NMR spectroscopy. The results of the 29si and 13C CP/MAS techniques were compared with the recently developed 1H MAS-only technique. Despite strong homonuclear dipole-dipole interactions it was possible to obtain well resolved 1H MAS spectra of those stationaru phases with a high degree of crosslinking. Limited mobility of the aromatic ligand fragments is common for all examined stationaryu phases. The chromatographic properties of the new phases were tested by their ability tio sepatate a mixture of eight PAHS. It could be shown that the π-π interaction mechanism is responsible for the separation of the eight PAHs, because the elution order of the PAHs did not changem despite the use of both a nonpolar mobile phase (n-heptane) and a polar mobile phase (methanol/ water mixture). 相似文献
97.
A new Fe(III)-imprinted amino-functionalized silica gel sorbent was prepared by a surface imprinting technique for selective solid-phase extraction (SPE) of Fe(III) prior to its determination by inductively coupled plasma atomic emission spectrometry (ICP-AES). Compared with non-imprinted polymer particles, the ion-imprinted polymers (IIPs) had higher selectivity and adsorption capacity for Fe(III). The maximum static adsorption capacity of the ion-imprinted and non-imprinted sorbent for Fe(III) was 25.21 and 5.10 mg g−1, respectively. The largest selectivity coefficient of the Fe(III)-imprinted sorbent for Fe(III) in the presence of Cr(III) was over 450. The relatively selective factor (αr) values of Fe(III)/Cr(III) were 49.9 and 42.4, which were greater than 1. The distribution ratio (D) values of Fe(III)-imprinted polymers for Fe(III) were greatly larger than that for Cr(III). The detection limit (3σ) was 0.34 μg L−1. The relative standard deviation of the method was 1.50% for eight replicate determinations. The method was validated by analyzing two certified reference materials (GBW 08301 and GBW 08303), the results obtained is in good agreement with standard values. The developed method was also successfully applied to the determination of trace iron in plants and water samples with satisfactory results. 相似文献
98.
Kizek R Masarik M Kramer KJ Potesil D Bailey M Howard JA Klejdus B Mikelova R Adam V Trnkova L Jelen F 《Analytical and bioanalytical chemistry》2005,381(6):1167-1178
The electroanalytical determination of avidin in solution, in a carbon paste, and in a transgenic maize extract was performed in acidic medium at a carbon paste electrode (CPE). The oxidative voltammetric signal resulting from the presence of tyrosine and tryptophan in avidin was observed using square-wave voltammetry. The process could be used to determine avidin concentrations up to 3 fM (100 amol in 3 l drop) in solution, 700 fM (174 fmol in 250 l solution) in an avidin-modified electrode, and 174 nM in a maize seed extract. In the case of the avidin-modified CPE, several parameters were studied in order to optimize the measurements, such as electrode accumulation time, composition of the avidin-modified CPE, and the elution time of avidin. In addition, the avidin-modified electrode was used to detect biotin in solution (the detection limit was 7.6 pmol in a 6 l drop) and to detect biotin in a pharmaceutical drug after various solvent extraction procedures. Comparable studies for the detection of biotin were developed using HPLC with diode array detection (HPLC-DAD) and flow injection analysis with electrochemical detection, which allowed biotin to be detected at levels as low as 614 pM and 6.6 nM, respectively. The effects of applied potential, acetonitrile content, and flow rate of the mobile phase on the FIA-ED signal were also studied. 相似文献
99.
用内径为0.53mm的填充毛细管正相液相色谱为第一维,用4.6mm(i.d.)×50mmRP-18e整体柱反相色谱为第二维,建立了定量环一阀切换接口的全二维液相色谱系统(NPLC×RPLC).第一维色谱分离洗脱出的组分交替存储在十通阀上的两个定量环中,同时定量环中前一个组分被转移到第二维进行反相分离.因为第一维的流动相流量仅是第二维的1/500,自然解决了流动相兼容问题.采用芳香族化合物的混合物和中药丹参正己烷提取液对该全二维液相系统的分离能力进行了评价. 相似文献
100.
Martínez-Pla JJ Martín-Biosca Y Sagrado S Villanueva-Camañas RM Medina-Hernández MJ 《Journal of chromatography. A》2004,1048(1):111-118
Capillary electrophoresis (CE) is a powerful technique for enantiomer separations due to its intrinsic high separation efficiencies, speed of analysis, low reagent consumption and small sample requirements. However, some chiral selectors present strong background UV absorption providing high detection limits. The present paper deals with the application of the partial-filling technique to the separation of bupivacaine enantiomers by capillary electrophoresis using human serum albumin (HSA) as chiral selector. In this procedure the cationic surfactant cetyltrimethylammonium bromide (CTAB) was used as a dinamic capillary coating in order to reduce the electro-osmotic flow and detect both bupivacaine enantiomers out of the chiral selector plug. Several experimental conditions such as CTAB concentration, pH, HSA concentration and plug length, background electrolyte concentration, temperature and voltage were studied. Under the selected conditions it is possible to detect the separated enantiomers out of the HSA plug in less than 4 min using 50 mM Tris pH 8 as background electrolyte with 50 microM CTAB, at 30 degrees C and using a separation voltage of 25 kV. The proposed methodology was then validated for analytical purposes and applied to the analysis of pharmaceutical preparations commercially available. The results obtained with the proposed methodology were in good agreement with those declared by the manufacturers. The simplicity, sample throughput, accuracy, reproducibility and low cost of the proposed method make it suitable for the control of the enantiomeric composition of bupivacaine in pharmaceuticals. 相似文献