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951.
Theoretical study of the effect of frit quality on chromatography using computational fluid dynamics
Summary Frits at both ends of a chromatographic column, especially for a preparative column, have significant influence on the flow
distribution within the column and thus the column efficiency. However, frits have received little attention from chromatographers
in the past. Here a theoretical study was conducted with the aid of CFD software FLUENT to investigate the effect of frits
on the performance of homogeneous and heterogeneous chromatographic columns. A dimensionless number,FQ, was applied to characterize frit quality. This study visualized how frit quality affects the flow distribution and the concentration
band, the shape of eluted pulse at the colum exit and column efficiency. Simulation results show that the development length
of the flow distribution is related toFQ but has nothing to do with the packing heterogeneity. The curvature of the concentration band in a column depends onFQ and packing quality. This study shows column efficiency can be improved significantly by increasingFQ and/or frit permeability. 相似文献
952.
TA-MS provides chemical and thermal response information. In order for this information to be meaningful sampling must be
performed with minimum dead volume and without cold spots. Dead volume leads to response lag and peak broadening. Cold spots
result in sample condensation, leading to inaccurate data and potentially inlet blockage. This paper describes a hot zone
inlet system and 'in-situ' probe both of which provide fast response, zero dead volume sampling directly to the MS. The paper
also discusses data interpretation methodologies and introduces 'soft ionisation' as a means of providing simplified analysis
of complex mixtures.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
953.
质谱在肽和蛋白质序列分析中的应用 总被引:7,自引:0,他引:7
了解肽和蛋白质的序列对理解其功能具有重要意义,测定其序列也是当前生命 科学研究中的重要内容之一,质谱作为高灵敏度的测定分子结构的仪器,其高灵敏 度、广泛的适用性及快速性等特性使它具有很大潜力发展成为辅助传统测序方法的 新方法,并得到了广泛的关注。从离子活化方法(包括碰撞诱导解离CID、源后裂 解PSD、源内裂解ISD等)、衍生化作用以及氨基酸残基消除方式(高能活化产生亚 稳离子、化学降解、酶降解)等多个角度介绍了利用质谱分析多肽和蛋白质序列的 方法,并对其发展前景作出展望。 相似文献
954.
Summary Two molecularly imprinted polymers (MIP) have been prepared using the acidic drug salicylic acid, which can form intramolecular
hydrogen bond, as the template and acrylamide or 4-vinylpyridine as the functional monomer. HPLC was used to evaluate the
binding performance of the MIP for the template and for several analogues. The results showed that the MIP (P2) prepared using acrylamide as the functional monomer had no molecular imprinting effect whereas that (P1) prepared using 4-vinylpyridine as the functional monomer had a significant molecular imprinting effect. The reason the molecular
imprinting effect was different for the two MIP was elucidated and the molecular recognition properties of P1 were studied in detail. It was confirmed that electrostatic interaction played an important role in the molecular recognition
of P1. Scatchard analysis showed that two types of binding site with distinctly different affinity were formed in P1. Their dissociation constants were estimated to be 7.6×10−5 mol L−1 and 3.2×10−3 mol L−1, respectively. Because P1 has high affinity and selectivity for salicylic acid not only in organic systems but also in water-containing systems, it
gives P1 the potential for use in the enrichment, separation, and detection of salicylic acid in biological fluids. 相似文献
955.
Glassy carbon electrodes modified with (5-amino-1,10-phenanthroline)bis(bipyridine)ruthium(II) chloride hydrate, [(bpy)2Ru(5-phenNH2)]Cl2·H2O, are shown to oxidize hydrazine with excellent sensitivity. The presence of an amine group on the ruthenium complex facilitates electropolymerization onto the electrode surface. Using cyclic voltammetry, a large catalytic current is observed upon oxidation of hydrazine in phosphate buffer (pH 5.0), compared to the current obtained from the ruthenium-modified electrode with no hydrazine present. The sensitivity of cyclic voltammetry is sufficient for obtaining a linear calibration curve for hydrazine over the range of 10−5 to 10−2 M. Hydrodynamic amperometry was used to determine the working potential for flow injection analysis. The limit of detection for hydrazine was determined to be 8.5 μM using FIA. The thickness of these films was shown to increase linearly with the number of electropolymerization cycles, in the range of 1000-2500 nm for 5-20 cycles, respectively, using Rutherford backscattering spectrometry (RBS). RBS analysis also suggests that the film is multilayered with the outermost layers containing a high ruthenium concentration, followed by layers where the concentration of ruthenium decreases linearly and approaches zero at the electrode surface. 相似文献
956.
在线固相萃取和高效液相色谱法测定卷烟主流烟气中几种芳胺 总被引:6,自引:1,他引:6
研究了用在线固相萃取富集和高效液相色谱法测定卷烟主流烟气中的几种芳胺(苯胺、对甲基苯胺、2,4-二甲基苯胺、1-萘胺、2-萘胺和4-氨基联苯)的方法,样品中的芳胺用邻甲氧基酚衍生生成偶氮染料,偶氮染料用WatersXterraTMRP18色谱柱在线固相萃取富集,然后以WatersXterraTMRP18色谱柱为固定相,75%的甲醇(内含0.01mol/LpH=8的四氢吡咯-醋酸缓冲液)为流动相分离,二极管矩阵检测器检测;苯胺、对甲基苯胺、2,4-二甲基苯胺、4-氨基联苯、1-萘胺、2-萘胺的检出限分别为005、0.08、0.08、0.06、0.03和0.03μg/L。几种芳胺的相对标准偏差在2.2%~3.4%之间;标准回收率在89%~106%之间,方法用于卷烟主流烟气中几种芳胺的测定,结果令人满意。 相似文献
957.
海洋生物体中稀土元素的微波消解电感耦合等离子体质谱测定研究 总被引:4,自引:0,他引:4
建立了微波消解样品处理、电感耦合等离子体质谱法测定海洋生物体中稀土元素的方法.用人发标准参考物质(GBW09101)、植物标准参考物质(GBW07603)以及实际样品标准加入回收的方法对文中所述的分析流程进行确认.实验结果表明,所建立方法的测定结果与标准参考物质的标准值或推荐值一致;样品标准加入实验的回收率在97%~104%之间.方法的定量下限为0.01~0.31 ng·g-1(10σ,n=10,干样). 相似文献
958.
动物尿液中盐酸克伦特罗的分子印迹固相萃取-气相色谱-质谱法研究 总被引:10,自引:0,他引:10
采用分子印迹聚合物(MIP)固相萃取小柱提取、净化并富集猪尿液中的盐酸克伦特罗分子,用N,O-双三甲基硅基三氟乙酰胺(BSTFA)衍生化,毛细管气相色谱-质谱联用(选择离子模式,选择离子为277、262、243和86)对衍生物分析。优化了MIP固相萃取柱的淋洗条件,考察了MIP固相萃取柱的净化效果和消除基体干扰能力,建立了对动物尿液中盐酸克伦特罗的定性、定量分析的方法。在优化条件下,本法检出限(LOD)为0.51μg/L,定量限(LOQ)为1.00μg/L;不同盐酸克伦特罗加入量的回收率为71.0%~89.3%;相对标准偏差为3.2%~9.7%。将该方法与农业行业标准方法比较,结果吻合较好。但该方法灵敏度和精密度高,操作更为简单、快捷。 相似文献
959.
960.
A rapid and reliable high performance liquid chromatographic (HPLC) method for the simultaneous determination of heterocyclic
compounds, namely nicotinic acid, nicotinamide, and 3-cyanopyridine, in industrial effluent is described. A Φ4.6 mm × 150
mm, 5 μm C-18 reversed phase stationery phase, and a methanol-acetonitrile-water tertiary mobile phase (20:20:60 v/v) were
used for separation. The detection wavelength of a diode array (DAD) was set at 216 nm with a bandwidth of 16 nm. Phenol was
used as an internal standard. The regression equations revealed a linear relationship between the concentration of the analytes
injected and the peak area detected by DAD. The limits of detection (S/N = 3) ranged from 0.70 to 1.18 mg L−1, the recoveries ranged from 87% to 102% and the precision expressed as % RSD intra-day and inter-day varied from 0.9 to 3.9
and 1.2 to 5.6, respectively. This method is rapid, sensitive and suitable for the monitoring of nicotinic acid, nicotinamide,
and 3-cyanopyridine in effluent of related pharmaceutical manufacturing plants. 相似文献