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Separation Column (separation + column)
Selected AbstractsDetermination of Reserpine in Urine by Capillary Electrophoresis with Electrochemiluminescence DetectionELECTROANALYSIS, Issue 3 2004Weidong Cao Abstract A fast and sensitive approach to detect reserpine in urine using micellar electrokinetic capillary chromatography with electrochemiluminescence (ECL) of Ru(bpy)32+ detection is described. Using a 25,,m i.d. capillary as separation column, the ECL detector was coupled to the capillary in the absence of an electric field decoupler. Field-amplified injection was used to minimize the effect of ionic strength in the sample and to achieve high sensitivity. In this way, the sample was analyzed directly without any pretreatment. The method was validated for reserpine in the urine over the range of 1×10,6,1×10,4,mol/L with a correlation coefficient of 0.996. The RSD for reserpine at a level of 5,,mol/L was 4.3%. The LOD (S/N=3) was estimated to be 7.0×10,8,mol/L. The average recoveries for 10,,mol/L reserpine spiked in human urine were 94%. [source] Underivatized cyclic olefin copolymer as substrate material and stationary phase for capillary and microchip electrochromatographyELECTROPHORESIS, Issue 15 2008Omar Gustafsson Abstract We report, for the first time, the use of underivatized cyclic olefin copolymer (COC, more specifically: Topas) as the substrate material and the stationary phase for capillary and microchip electrochromatography (CEC), and demonstrate chromatographic separations without the need of coating procedures. Electroosmotic mobility measurements in a 25,,m id Topas capillary showed a significant cathodic EOF that is pH-dependent. The magnitude of the electroosmotic mobility is comparable to that found in glass substrates and other polymeric materials. Open-tubular CEC was employed to baseline-separate three neutral compounds in an underivatized Topas capillary with plate heights ranging from 5.3 to 12.7,,m. The analytes were detected using UV absorbance at 254,nm, thus taking advantage of the optical transparency of Topas at short wavelengths. The fabrication of a Topas-based electrochromatography microchip by nanoimprint lithography is also presented. The microchip has an array of pillars in the separation column to increase the surface area. The smallest features that were successfully imprinted were around 2,,m wide and 5,,m high. No plasma treatment was used during the bonding, thus keeping the surface properties of the native material. An RP microchip electrochromatography separation of three fluorescently labeled amines is demonstrated on the underivatized microchip with plate heights ranging from 3.4 to 22,,m. [source] Speciation of selenium compounds by open tubular capillary electrochromatography-inductively coupled plasma mass spectrometryELECTROPHORESIS, Issue 21 2006Shu-Yu Lin Abstract We introduce a T-type interface and a crossflow nebulizer to find ways to combine CEC with inductively coupled plasma MS (ICP-MS) detection for selenium speciation. For CEC separation, we employed a macrocyclic polyamine-bonded phase capillary as the separation column and a bare fused-silica capillary filled with the make-up liquid (0.05,M,HNO3). The effect of nebulizer gas flow rate, make-up liquid flow, type, concentration and pH of the mobile phase on the separation have been studied. Tris buffer of 50,mM at pH,8.50 gave the best performance for selenium speciation. The reproducibility of the retention time indicated that sample injection by electrokinetic and nebulizer gas flow was better than that by self-aspiration alone. The detection limits for selenate, selenite, selenocystine and selenomethionine were found to be 2.40, 3.53, 12.86 and 11.25,ng/mL, respectively. Due to the high sensitivity and element-specific detection, as well as the high selectivity of the bonded phase, quantitative analysis of selenium speciation in urine was also achieved. [source] Analyses of preservatives by capillary electrochromatography using methacrylate ester-based monolithic columnsELECTROPHORESIS, Issue 18-19 2004Hsi-Ya Huang Abstract Five common food preservatives were analyzed by capillary electrochromatography, utilizing a methacrylate ester-based monolithic capillary as separation column. In order to optimize the separation of these preservatives, the effects of the pore size of the polymeric stationary phase, the pH and composition of the mobile phase on separation were examined. For all analytes, it was found that an increase in pore size caused a reduction in retention time. However, separation performances were greatly improved in monolithic columns with smaller pore sizes. The pH of the mobile phase had little influence on separation resolution, but a dramatic effect on the amount of sample that was needed to be electrokinetically injected into the monolithic column. In addition, the retention behaviors of these analytes were strongly influenced by the level of acetonitrile in the mobile phase. An optimal separation of the five preservatives was obtained within 7.0 min with a pH 3.0 mobile phase composed of phosphate buffer and acetonitrile 35:65 v/v. Finally, preservatives in real commercial products, including cold syrup, lotion, wine, and soy sauces, were successfully determined by the methacrylate ester-based polymeric monolithic column under this optimized condition. [source] Detection and validated quantification of nine herbal phenalkylamines and methcathinone in human blood plasma by LC-MS/MS with electrospray ionizationJOURNAL OF MASS SPECTROMETRY (INCORP BIOLOGICAL MASS SPECTROMETRY), Issue 2 2007Jochen Beyer Abstract The herbal stimulants Ephedra species, Catha edulis (khat), and Lophophora williamsii (peyote) have been abused for a long time. In recent years, the herbal drug market has grown owing to publicity on the Internet. Some ingredients of these plants are also ingredients of cold remedies. The aim of the presented study is to develop a multianalyte procedure for detection and validated quantification of the phenalkylamines ephedrine, pseudoephedrine, norephedrine, norpseudoephedrine, methylephedrine, methylpseudoephedrine, cathinone, mescaline, synephrine (oxedrine), and methcathinone in plasma. After mixed-mode solid-phase extraction of 1 ml of plasma, the analytes were separated using a strong cation exchange separation column and gradient elution. They were detected using a Q-Trap LC-ESI-MS/MS system (MRM mode). Calibration curves were used for quantification using norephedrine- d3, ephedrine- d3, and mescaline- d9 as internal standards. The method was validated according to international guidelines. The assay was selective for the tested compounds. It was linear from 10 to 1000 ng/ml for all analytes. The recoveries were generally higher than 70%. Accuracy ranged from , 0.8 to 20.0%, repeatability from 2.5 to 12.3%, and intermediate precision from 4.6 to 20.0%. The lower limit of quantification was 10 ng/ml for all analytes. No instability was observed after repeated freezing and thawing or in processed samples. The applicability of the assay was tested by analysis of authentic plasma samples after ingestion of different cold medications containing ephedrine or pseudoephedrine, and after ingestion of an aqueous extract of Herba Ephedra. After ingestion of the cold medications, only the corresponding single alkaloids were detected in human plasma, whereas after ingestion of the herb extract, all six ephedrines contained in the plant were detected. The presented LC-MS/MS assay was found applicable for sensitive detection and accurate and precise quantification of all studied analytes in plasma. Copyright © 2006 John Wiley & Sons, Ltd. [source] Simple sample transfer technique by internally expanded desorptive flow for needle trap devicesJOURNAL OF SEPARATION SCIENCE, JSS, Issue 12 2008In-Yong Eom Abstract Needle trap devices (NTDs) are improving in simplicity and usefulness for sampling volatile organic compounds (VOCs) since their first introduction in early 2000s. Three different sample transfer methods have been reported for NTDs to date. All methods use thermal desorption and simultaneously provide desorptive flow to transfer desorbed VOCs into a GC separation column. For NTDs having ,side holes', GC carrier gas enters a ,side hole' and passes through sorbent particles to carry desorbed VOCs, while for NTD not having a ,side hole', clean air as desorptive flow can be provided through a needle head by a air tight syringe to sweep out desorbed VOCs or water vapor has been reported recently to be used as desorptive flow. We report here a new simple sample transfer technique for NTDs, in which no side holes and an external desorptive flow are required. When an NTD enriched by a mixture of benzene, toluene, ethylbenzene, and xylene (BTEX) or n -alkane mixture (C6,C15) is exposed to the hot zone of GC injector, the expanding air above the packed sorbent transfers the desorbed compounds from the sorbent to the GC column. This internal air expansion results in clean and sharp desorption profiles for BTEX and n -alkane mixture with no carryover. The effect of desorption temperature, desorption time, and overhead volumes was studied. Decane having vapor pressure of ,1 Torr at 20°C showed ,1% carryover at the moderate thermal desorption condition (0.5 min at 250°C). [source] On-line concentration and pressurized capillary electrochromatographic analysis of phytohormones in cornJOURNAL OF SEPARATION SCIENCE, JSS, Issue 5 2008Shujuan Wang Abstract A pressurized CEC (pCEC) method was developed for the separation of phytohormones, in which UV absorbance was used as the detector and a monolithic silica-ODS column as the separation column. The parameters (including the concentration of organic solvent in the mobile phase, pH of the electrolyte buffer, applied voltage) affecting the separation resolution were evaluated. Two on-line concentration techniques, namely, solvent gradient zone sharpening effect and field-enhanced sample stacking, were utilized to improve detection sensitivity. The combination of the two techniques proved to be beneficial to enhance the detection sensitivity by enabling the injection of large volumes of samples. Compared to the conventional injection mode, the enhancement in the detection sensitivities of phytohormones using the on-line concentration technique is in the range from 9- to 23-fold. The developed pCEC method was applied to evaluate phytohormones in corns. [source] Determination of bisphenol A in rat brain by microdialysis and column switching high-performance liquid chromatography with fluorescence detectionBIOMEDICAL CHROMATOGRAPHY, Issue 5 2002Yen Sun A sensitive column switching HPLC-fluorescence detection for determination of bisphenol A (BPA) in rat brain by coupling with microdialysis was developed. A microdialysis probe was inserted into the hypothalamus of rat brain and an artificial cerebrospinal fluid was used for perfusion. BPA in brain dialysate was subjected to a fluorescent derivatization with 4-(4,5-diphenyl-1H -imidazol-2-yl)benzoyl chloride (DIB-Cl), and the excess reagent was removed by a column-switching technique. Separation was carried out on two ODS semimicro-columns with the mobile phase of acetonitrile,H2O,methanol,tetrahydrofuran (55:10:35:2.5, v/v) and acetonitrile,0.1,M acetate buffer (pH 3.0),methanol (35:10:55, v/v) at a flow rate of 0.10 and 0.15,mL/min for a precolumn and a separation column, respectively. Fluorescence intensity was monitored at 475,nm with excitation of 350,nm. BPA could be sensitively detected at 0.3 ppb in 60,µL brain microdialysate at a signal-to-noise ratio of 3. By the proposed method, concentrations of BPA in rat brain and plasma were monitored for 8,h after single i.v. or oral administration. It is proved that BPA is capable of penetrating the blood,brain barrier. The ratio of the area under the concentration,time curve of BPA in rat brain to that in blood was estimated to be about 3.0,3.8%. Copyright © 2002 John Wiley & Sons, Ltd. [source] Monolithic media in microfluidic devices for proteomicsELECTROPHORESIS, Issue 18 2006Kyung Won Ro Abstract Considerable effort has been invested in the development of integrated microfluidic devices for fast and highly efficient proteomic studies. Among various fabrication techniques for the preparation of analytical components (separation columns, reactors, extractors, valves, etc.) in integrated microchips, in situ fabrication of monolithic media is receiving increasing attention. This is mainly due to the ease and simplicity of preparation of monolithic media and the availability of various precursors and chemistries. In addition, UV-initiated photopolymerization technique enables the incorporation of multiple analytical components into specified parts of a single microchip using photomasks. This review summarizes preparation methods for monolithic media and their application as microfluidic analytical components in microchips. [source] Preparing titania aerogel monolithic chromatography columns using supercritical carbon dioxideJOURNAL OF SEPARATION SCIENCE, JSS, Issue 11 2010Ruohong Sui Abstract The search for a method to fabricate monolithic inorganic columns has attracted significant recent attention due to their unique ability in separation applications of various biomolecules. Silica and polymer based monolithic columns have been prepared, but titania and other metal oxide monoliths have been elusive, primarily due to their fragility. This article describes a new approach for preparing nanostructured titania based columns, which offer better performance over conventional particle packed columns for separating a wide variety of biomolecules including phosphopeptides. TiO2 monolithic aerogels were synthesized in separation columns using in situ sol-gel reactions in supercritical carbon dioxide (scCO2) followed by calcination, and compared to those prepared in heptanes. The characterization results show that scCO2 is a better solvent for the sol-gel reactions, providing lower shrinkage with the anatase TiO2 monolith composed of nanofibers with very high surface areas. The monolithic columns show the ability to isolate phosphopeptides with little flow resistance compared to conventional titania particle based microcolumns. [source] Separation of benzene and deuterated benzenes by reversed-phase and recycle liquid chromatography using monolithic capillary columnsJOURNAL OF SEPARATION SCIENCE, JSS, Issue 15-16 2004Lee Wah Lim Abstract An alternate pumping-recycle system utilizing a commercially available low dead-volume switching valve was developed for microcolumn LC. The recycle system had two separation columns, and the dead volume of the recycling lines was kept to a minimum by avoiding passage of the sample through the pump chamber, sample injector, and the normal path length of a conventional UV detector. The drawback of the high total back pressure caused by the second column that is placed after the detector was overcome by on-column detection, and this eliminated the need for a high pressure flow cell. The system was used for the separation of an authentic mixture of benzene, benzene-1,3,5-d3, and benzene-d6. Baseline separation was accomplished after six cycles and the calculated theoretical plate number for benzene was 230,000. It was observed that the theoretical plate number (N) increased linearly with increasing number of cycles, and the N per unit time increased with increasing inlet pressure. The separation conditions were optimized and the separation of benzene and benzene-d6 was accomplished within 75 min at 2.5 MPa inlet pressure. [source] | ||||||||||