The Synthesis and Characterization of Reversed Phase Stationary Phases for High Performance Liquid Chromatography PDF Download
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Author: Karen Wink Barnes
Publisher:
ISBN:
Category : High performance liquid chromatography
Languages : en
Pages : 324
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Book Description
Reversed phase liquid chromatography (RPLC) is a widely used separation technique today. The stationary phase, composed of hydrocarbon moieties chemically bound to a silica support, is commonly prepared by refluxing the silica with a reactive silane in an appropriate solvent. Siloxane bonds, Si-O-Si, are formed. There are limitations to RPLC in that nonhomogeneous surface coverages, detrimental to efficient separations, result from the bonding process, and because the reaction is never complete due to steric restrictions. Also, silica is soluble at high pH values, and the Si-C bond binding the hydrocarbon to the silica is labile at low pH ranges. Thus, the usable pH range for silica stationary phases is 2.5 to 7.5, and often this range is too narrow to allow the separation of a mixture. The use of ultrasonic cavitation to catalyze silane bonding was investigated to dtermine whether the vigorous ultrasonic process would drive reagents into the surface pores and better distribute the hydrocar bonaceous reagent, thereby producing a more efficient stationary phase. Tandem reactions proved that ultrasonic bonding procedures are as effective as the refluxed, and that the chromatographic efficiency of the ultrasonic phases was comparable, if not superior, to the refluxed. Chromatographic tests also indicated the ultrasonic phases were comparable to commercially available phases. The reproducibility of the reactions and the effect of acoustic power and heat were also investigated. A second set of experiments investigated substitution of alumina for silica because the alumina crystalline structure remains intact over a pH range of 2 to 12. A trifunctional modification scheme generating a thick cross-linked hydrocarbon matte was used because the Al-0 bond is susceptible to hydrolysis, which strips the bound hydrocarbons, by polar RP solvents. Five aluminas were bonded and tested for chromatographic utility. Reaction conditions were optimized, and ultrasonic bonding was investigated. It was found that alumina with a sufficiently active surface is modifiable, and that the modified surface is remarkably stable for use with acidic and basic buffers and in neutral, polar solvent mixtures. The chromatographic utility of alumina phases was demonstrated and compared with the silica results.
Author: Karen Wink Barnes
Publisher:
ISBN:
Category : High performance liquid chromatography
Languages : en
Pages : 324
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Book Description
Reversed phase liquid chromatography (RPLC) is a widely used separation technique today. The stationary phase, composed of hydrocarbon moieties chemically bound to a silica support, is commonly prepared by refluxing the silica with a reactive silane in an appropriate solvent. Siloxane bonds, Si-O-Si, are formed. There are limitations to RPLC in that nonhomogeneous surface coverages, detrimental to efficient separations, result from the bonding process, and because the reaction is never complete due to steric restrictions. Also, silica is soluble at high pH values, and the Si-C bond binding the hydrocarbon to the silica is labile at low pH ranges. Thus, the usable pH range for silica stationary phases is 2.5 to 7.5, and often this range is too narrow to allow the separation of a mixture. The use of ultrasonic cavitation to catalyze silane bonding was investigated to dtermine whether the vigorous ultrasonic process would drive reagents into the surface pores and better distribute the hydrocar bonaceous reagent, thereby producing a more efficient stationary phase. Tandem reactions proved that ultrasonic bonding procedures are as effective as the refluxed, and that the chromatographic efficiency of the ultrasonic phases was comparable, if not superior, to the refluxed. Chromatographic tests also indicated the ultrasonic phases were comparable to commercially available phases. The reproducibility of the reactions and the effect of acoustic power and heat were also investigated. A second set of experiments investigated substitution of alumina for silica because the alumina crystalline structure remains intact over a pH range of 2 to 12. A trifunctional modification scheme generating a thick cross-linked hydrocarbon matte was used because the Al-0 bond is susceptible to hydrolysis, which strips the bound hydrocarbons, by polar RP solvents. Five aluminas were bonded and tested for chromatographic utility. Reaction conditions were optimized, and ultrasonic bonding was investigated. It was found that alumina with a sufficiently active surface is modifiable, and that the modified surface is remarkably stable for use with acidic and basic buffers and in neutral, polar solvent mixtures. The chromatographic utility of alumina phases was demonstrated and compared with the silica results.
Author: Karen Wink Barnes
Publisher:
ISBN:
Category : High performance liquid chromatography
Languages : en
Pages : 0
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Book Description
Author: Dale Allen Shoemaker
Publisher:
ISBN:
Category :
Languages : en
Pages : 210
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Book Description
Author: Niloofar Salehi
Publisher:
ISBN:
Category : High performance liquid chromatography
Languages : en
Pages : 129
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Book Description
High pressure liquid chromatography is one of the most frequently used methods for the separation of mixtures. Chemically modified silica hydride stationary phases, due to their unique selectivity and versatility, have been the focus of an increasing number of studies in the past several years. The objective of fabricating stationary phases with dual properties is to achieve separation of both polar and non-polar components in a single analysis. Due to an increasing demand in the fields of drug discovery, proteomics, and metabolomics to analyze numerous samples with a wide range of polarities, there is a need for more versatile stationary phases for a wide range of applications. In order to meet the above objective, in this research four novel silica hydride-based columns were synthesized using a hydrosilation procedure. The characterization of each column was done using a series of polar and nonpolar compounds by studying their aqueous normal phase and reversed-phase chromatographic behavior. Under these conditions, it turned out that two columns showed both RP and ANP behaviors. Of the remaining columns, one exhibited ANP behavior only and the other performed only in the reversed-phase mode.
Author: Steven Douglas Fazio
Publisher:
ISBN:
Category : Chromatographic analysis
Languages : en
Pages : 392
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Book Description
Author: Zhuxu Wang
Publisher:
ISBN:
Category : Chemical bonds
Languages : en
Pages : 124
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Book Description
Author: Louis W. Yu
Publisher:
ISBN:
Category : Aldehydes
Languages : en
Pages : 450
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Book Description
Author: David S. Van Meter (III.)
Publisher:
ISBN:
Category :
Languages : en
Pages : 179
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Book Description
Author: Stavros Kromidas
Publisher: John Wiley & Sons
ISBN: 3527336818
Category : Science
Languages : en
Pages : 378
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Book Description
The rapid development of HPLC instrumentation and technology opens numerous possibilities - and entails new questions. Which column should I choose to obtain best results, which gradient fits to my analytical problem, what are recent and promising trends in detection techniques, what is state of the art regarding LC-MS coupling? All these questions are answered by experts in ten self-contained chapters. Besides these more hardware-related and technical chapters, further related areas of interest are covered: Comparison of recent chromatographic data systems and integration strategies, smart documentation, efficient information search in internet, and tips for a successful FDA inspection. This practical approach offers in a condensed manner recent trends and hints, and will also display the advanced reader mistakes and errors he was not aware of so far.
Author: Asanka Wijekoon
Publisher:
ISBN:
Category : High performance liquid chromatography
Languages : en
Pages : 274
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Book Description
High performance liquid chromatography is a powerful analytical technique employed to separate analyte mixtures. Since biomedical sample mixtures contain a very diverse range of compounds; one chromatographic mode is usually unable to separate all components of the mixture. Therefore, there is an increasing need for faster and efficient separations with a broad range of selectivity. To attain better selectivity and efficient separation, and to improve the versatility of the chromatographic column, a new way of preparation of multifunctional stationary phases, suitable for use in multiple chromatographic separation modes, is described. The preparation of multifunctional stationary phases takes advantage of Schiff base chemistry in two different synthetic routes. The first route involves reductive coupling of amino bonded silica with aldehyde containing ligands. The coupling of aldehyde bonded silica with amine containing ligands is the other reaction route. Aldehyde terminated silica is a versatile reactive platform that enables the synthesis of a wide range of stationary phases by attaching amine containing ligands that have diverse functionality. Here the preparation of aldehyde terminated silica was achieved by bonding aldehyde silane to the silica surface. Preparation of aldehyde silane is a novel approach and a successful synthetic scheme of making acetalated aromatic aldehyde silane (AAS- Aldehyde group in the silane has been protected by acetalation) and aromatic aldehyde silane (AS) is invented. The studies confirmed that the synthesized multifunctional chromatographic stationary phases were capable of operating in ion exchange mode, reversed phase mode and hydrophilic interaction liquid chromatographic mode. The studies further concluded that those surfaces have good selectivity for the separation of small polar and charge molecules. The application of the well established Schiff base reaction allowed the incorporation 2H to the bonded phases and is utilized to study the motional dynamics of the bonded ligands in the surface at different temperatures in the presence of a broad range of solvent systems by using 2H wide line NMR spectroscopy. The investigation provides information about the motional dynamic heterogeneity of the bonded ligands, which reflects the existence of surface heterogeneity of the surface.
