Preparation and evaluation of slurry-packed capillary columns for normal-phase liquid chromatography

This review discusses many different aspects of microcolumn liquid chromatography (LC) and reflects the areas of microcolumn LC research interest over the past decades. A brief theoretical discussion on a number of major issues, such as column characterisation, chromatographic dilution effects and extracolumn band broadening in microcolumn LC is given. Recent progress in column technology and the demands and developments of instrumentation and accessories for microcolumn LC are also reviewed. Besides that, the developments in a large number of established and also more recent detection techniques for microcolumn LC are also discussed. The potential of hyphenation of microcolumn LC with other techniques, more particularly of multidimensional chromatography and microcolumn LC coupled to mass spectrometry is reviewed. Finally, the perspective of microcolumn LC separation methods is stressed by a number of relevant applications.

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“…[76][77][78][79][80][81][82]), but also by column parameters (such as column blank material, frit selection, etc. [76,[83][84][85][86]).…”

Section: Column Developmentsmentioning

confidence: 99%

Microcolumn liquid chromatography: instrumentation, detection and applications

Vissers¹,

Claessens

Cramers

1997

Journal of Chromatography A

208

101

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“…It should be pointed out that the diol column shows a better column performance than the cyano columns, even though h-, is slightly higher, because of its good permeability. If the data are compared again with those of Andreolini et al [8], similar data are obtained for 4, h-, and E. As an example, the data obtained for dimethylphthalate are tabulated. Figure 5 shows the reduced van Deemter plot for dimethylphthalate and 1,3-dinitrobenzene on a silica packing.…”

Section: Resultsmentioning

confidence: 68%

Liquid chromatography capillary columns dry‐packed with polar and nonpolar stationary phases

Crescentini

Mastrogiacomo

1991

J Microcolumn Separations

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Abstract. Fused silica capillary columns of 0.250-mm i.d., packed with 5-pm particles of nonpolar (octadecyl, octyl, and butyl) and polar (silica, diol, cyano, and amino) materials, have been prepared using a dry-packing technique. The performance of the columns has been evaluated using the reduced plate heightlreduced velocity equation and the separation impedance values. A comparison with similar slurry-packed columns shows that the dry-packing method may yield, in most cases, columns of analogous or better efficiency and requires a simpler apparatus and a shorter time for column preparation.

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“…; 360 μm o.d. ; Polymicro Technologies, Phoenix, AZ) against Microtight filter assemblies (Upchurch Scientific, Oak Harbor, WA) [34–36]. The same filter assemblies were used as retaining frits at the column inlet.…”

Section: Methodsmentioning

confidence: 99%

Highly stabilized, polymer–lipid membranes prepared on silica microparticles as stationary phases for capillary chromatography

Gallagher

Adem

Baker

et al. 2015

Journal of Chromatography A

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The ability to rapidly screen complex libraries of pharmacological modulators is paramount to modern drug discovery efforts. This task is particularly challenging for agents that interact with lipid bilayers or membrane proteins due to the limited chemical, physical, and temporal stability of conventional lipid-based chromatographic stationary phases. Here, we describe the preparation and characterization of a novel stationary phase material composed of highly stable, polymeric-phospholipid bilayers self-assembled onto silica microparticles. Polymer lipid membranes were prepared by photochemical or redox initiated polymerization of 1,2-bis[10-(2′,4′-hexadieoyloxy)decanoyl]-sn-glycero-2-phosphocholine (bis-SorbPC), a synthetic, polymerizable lipid. The resulting polymerized bis-SorbPC (poly(bis-SorbPC)) stationary phases exhibited enhanced stability compared to particles coated with 1,2-dioleoyl-sn-glycero-phosphocholine (unpolymerized) phospholipid bilayers when exposed to chemical (50mM triton X-100 or 50% acetonitrile) and physical (15 min sonication) insults after 30 days of storage. Further, poly(bis-SorbPC)-coated particles survived slurry packing into fused silica capillaries, compared to unpolymerized lipid membranes, where the lipid bilayer was destroyed during packing. Frontal chromatographic analyses of the lipophilic small molecules acetylsalicylic acid, benzoic acid, and salicylic acid showed > 44% increase in retention times (P < 0.0001) for all analytes on poly(bis-SorbPC)-functionalized stationary phase compared to bare silica microspheres, suggesting a lipophilic retention mechanism. Phospholipid membrane-functionalized stationary phases that withstand the chemical and physical rigors of capillary LC conditions can substantially increase the efficacy of lipid membrane affinity chromatography, and represents a key advance towards the development of robust membrane protein-functionalized chromatographic stationary phases.

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Preparation and evaluation of slurry-packed capillary columns for normal-phase liquid chromatography

Cited by 40 publications

References 19 publications

Microcolumn liquid chromatography: instrumentation, detection and applications

Microcolumn liquid chromatography: instrumentation, detection and applications

Liquid chromatography capillary columns dry‐packed with polar and nonpolar stationary phases

Highly stabilized, polymer–lipid membranes prepared on silica microparticles as stationary phases for capillary chromatography

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