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71.
A high sensitivity, multichannel fluorescence detector with small volume has been developed for capillary column liquid chromatography. Using an intensified linear photodiode array to monitor fluorescence emission, several important mixtures exhibiting native fluorescence have been examined following high efficiency separation on a capillary column. By correlating mass spectral, fluorescence spectral, and retention time data, information of potential utility in the structural elucidation of aromatic molecules contained in complex mixtures can be obtained. Examples include the separation and spectral examination of the polyaromatic compounds in samples of both biological and environmental interest. 相似文献
72.
十二烷基硫酸钠毛细管电泳法因具有快速、分辨率高的优势,已成为单克隆抗体纯度分析的主流方法。在非还原单克隆抗体纯度检测中,其样品前处理过程对于结果有显著影响。为优化样品前处理,考察了以碘乙酰胺和N-乙基马来酰亚胺为巯基封闭剂,在pH 6.0~9.0的样品缓冲液条件下,不同种类和批次的单抗的纯度。发现在两种巯基封闭剂中,高pH的样品缓冲液会影响巯基封闭的效果,产生较多的抗体片段;而在低pH条件下,抗体片段较少,单抗的纯度更高。因此在进行非还原单抗的纯度检测中,pH 6.0的样品缓冲液为最佳的前处理条件。 相似文献
73.
G. V. Kotelnikov Sophia P. Moiseyeva E. V. Mezhburd E. I. Maevsky Elena V. Grishina 《Journal of Thermal Analysis and Calorimetry》2005,81(2):255-259
Summary Measurements of energy transformation in mitochondria are done on a capillary differential titration calorimeter CTD2156. It is important to mention that a sediment is quickly formed by the mitochondria suspension without mixing by means of a vibrating needle. During the measurements, the vibrating needle is located inside the working volume of the chamber. The design of the calorimeter is substantiated theoretically. It provides a new mode of a reagent input in the measuring volume of the calorimetric chambers. It expands the spectrum of tasks that can be solved using this instrument. In the capillary calorimeter the calorimetric chambers unit is simple and small in size. These advantages of capillary chambers provide an opportunity to unite 20 capillary calorimetric chambers in one calorimetric block. It allows designing a multi-channel titration calorimeter. There are obvious advantages of such a calorimeter over other instruments in screening researches and in researches of objects maintaining stability only for a short time. 相似文献
74.
75.
Polyethylene glycols can be immobilized in glass capillary columns by a new procedure involving covering the glass walls with a layer of graphitized carbon black and by flowing a mixture of the stationary phase and dicumyl peroxide. After curing and conditioning the column is ready for use. Excellent performance is reported for Carbowax 20 M and high molecular weight glycols. For other glycols the immobilized layer is less stable and can be washed out. 相似文献
76.
建立了高效毛细管电泳拆分阿苯达唑亚砜对映体的方法,考察了背景电解质pH、环糊精种类和浓度,有机改性剂种类和浓度对分离的影响,对分离条件进行了优化。实验结果表明:在含36g/L磺化β-环糊精和10%甲醇的20mmol/L Tris-H3PO4(pH2.5)缓冲体系中,阿苯达唑亚砜对映体具有良好的分离效果。 相似文献
77.
P. Torline G. du Plessis N. Schnautz J. C. Thompson 《Journal of separation science》1979,2(10):613-616
A detailed method for the routine preparation of glass capillary columns is presented. The method consists of coating a glass tube with quartz powder prior to pulling the tube into a capillary. The inner surface of the capillary consists of an even distribution of quartz particles fused to the walls. This surface has been found readily deactivated by standard procedures and ideal for the preparation of thick-film glass capillary columns. The method has been thoroughly tested in two independent laboratories to ensure that the procedures described are reproducible. 相似文献
78.
J. Miguel Vadillo M. Esther Gonzalez Isabel Carretero J. Javier Laserna 《Mikrochimica acta》1995,118(3-4):273-282
Micellar liquid chromatography (MLC) and capillary zone electrophoresis (CZE) have been evaluated for the analysis of twelve banned drugs in sport including diuretics and -blockers. In MLC, a sodium dodecylsulphate aqueous solution has been used as mobile phase using an octadecylsilica column. In CZE, a pH 8 buffer solution and a silica capillary have been employed. Parameters of retention and efficiency have been compared. Limits of detection with UV detection at 254 nm and relative standard deviations for atenolol, furosemide, nadolol, spironolactone and triamterene were established and compared in both techniques. Examples of direct urine injection into the separation systems are presented. Drugs overlapping in MLC are well resolved in CZE, while the opposite is true for a limited number of drugs. Some interferences from urine may arise in CZE. The selectivity of analysis would be greatly enhanced by using both techniques, which require only filtration as pre-treatment. 相似文献
79.
Summary Retention indices of 6 selected hydroxy compounds (aliphatic and bicyclic alcohols, phenols) were determined on 2 HP-5 fused-silica, capillary columns with different film thicknesses (0.11 m and 0.33 m) at 8 different oven temperatures between 80 and 150°C. For some substances the I-T plot was found to show a minimum which cannot be explained by the common retention-index temperature-dependence in gas-liquid chromatography. This result is discussed in terms of adsorption at the liquid-solid interface of the capillary column. 相似文献
80.
The values of partial molar free energy (G), enthalpy (H), and entropy (S) of sorption in the homologous series ofN-alkylpiperidines,N-alkylmorpholines,N-alkyl thiomorpholines, and alkylcyclohexanes were determined. It was found that the free energy of sorption is determined to a greater extent by the enthalpy term than by the entropy one. The free energy of sorption of the first homolog decreases when then-alkyl chain is attached directly to the carbon atom of the cycle and increases in the case ofN-alkylsubstituted heterocycles. The influence of the heteroatom nature on intermolecular interactions of homologs with the nonpolar stationary phase was quantitatively estimated on the basis of thermodynamic data.Dead time necessary for calculation of the retention factor was determined by the retention of methane injected into the column simultaneously with the sample.Translated from Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 2030–2032, August, 1996. 相似文献