On-column preparation of bonded phases for high pressure liquid chromatography

Gilpin, R. K.; Korpi, J.; Janicki, Casimir A.

doi:10.1021/ac60345a029

Cited by 34 publications

(15 citation statements)

References 18 publications

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“…Teflon-lined stainless steel and regular stainless steel columns 2 f t in length, by a combination of suction and gentle vibration. (Initially (15) only Teflon-lined stainless steel tubing was used. In this work, however, no significant difference was observed by using regular stainless steel tubing.)…”

Section: Methodsmentioning

confidence: 99%

“…Hastings et al (7) have described a partial insitu process in which the final polymerization was carried out directly in the column. Later, Gilpin and coworkers (14,15) discussed a simple, totally in-situ process for preparing bonded phases for HPLC use. Columns were prepared by the reaction of either octadecyltrichlorosilane or phenyltrichlorosilane with porous layer silica beads (Corasil 11, 37-50 p).…”

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In-situ chemically bonded stationary phases for high pressure liquid chromatography

Gilpin¹,

Korpi²,

Janicki³

1975

Anal. Chem.

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Chemically bonded stationary phases for high pressure Iiquld chromatography (HPLC) have been used In a variety of applications. In previous work, we have described a slmpie and totally In-situ process for preparing bonded phases for high pressure iiquld chromatographic use. Columns were prepared by reaction of either octadecyltrichlorosllane or phenyltrlchiorosllane with porous layer slilca beads. Inltlaliy, pre-reaction surface moisture was controlled by drying with flowing nitrogen. However, the performance and reproducibility of bonded phase packings are controlled to a large degree by the amount of bonded material on the surface. Since the trlchlorosilanes used polymerire readily In the presence of moisture, the amount of material bonded to the silica surface can easily vary between different columns unless the amount of water Is controlled to a reproducible degree. This paper describes a set of In-situ reaction condltlons which produce columns with a better degree of reproducibility. The amount of physically adsorbed surface water was established by first pumping water-saturated toluene followed by a specified volume of dry toluene through packed columns. In addition to discussing the actual preparation technique, the general chromatographic behavior of several In-situ prepared columns has been examined.Chemically bonded stationary phases for high pressure liquid chromatography (HPLC) have been used in a variety of applications. The most familiar means of preparing these phases is by bonding various organosilane molecules to a silica type surface. Perhaps the most common of these have been the reactions of the chlorosilanes. Chlorosilanes react with surface hydroxyl groups to form bonded films of varying structure (1). A number of adsorbent modification procedures employing di-and trichlorosilanes have been used to form bonded phases for chromatographic use ( I -16).Previously several workers have described in-situ processes for preparing bonded phases for chromatographic application. Hastings et al. (7) have described a partial insitu process in which the final polymerization was carried out directly in the column. Later, Gilpin and coworkers (14,15) discussed a simple, totally in-situ process for preparing bonded phases for HPLC use. Columns were prepared by the reaction of either octadecyltrichlorosilane or phenyltrichlorosilane with porous layer silica beads (Corasil 11, 37-50 p). Advantages of the method were ease and convenience of preparation.One of the most important factors affecting the performance of bonded phase columns is the amount of material deposited on the surface (8). Since the trichlorosilanes used polymerize readily in the presence of moisture, the amount of material bonded to the silica surface can easily vary between different columns unless the amount of water is controlled to a reproducible degree.This paper describes a set of in-situ reaction conditions which produce columns with a good degree of reproducibilAuthor to whom correspondence should be addressed.ity. In addition, several...

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Section: Methodsmentioning

confidence: 99%

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confidence: 99%

In-situ chemically bonded stationary phases for high pressure liquid chromatography

Gilpin¹,

Korpi²,

Janicki³

1975

Anal. Chem.

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“…Modern column selection, classification, characterization tests, and systems have evolved from the early works of Buszewski, − Engelhardt, − Euerby, − Gilpin, − Guiochon, − Horvath, ,,,− Jandera, − Kirkland, − Le Mahipan, − Majors, − Neue, − Sander and Wise, − Snyder, − Tanaka, − …”

Section: Introductionmentioning

confidence: 99%

Column Characterization and Selection Systems in Reversed-Phase High-Performance Liquid Chromatography

et al. 2019

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Reversed-phase high-performance liquid chromatography (RP-HPLC) is the most popular chromatographic mode, accounting for more than 90% of all separations. HPLC itself owes its immense popularity to it being relatively simple and inexpensive, with the equipment being reliable and easy to operate. Due to extensive automation, it can be run virtually unattended with multiple samples at various separation conditions, even by relatively low-skilled personnel. Currently, there are >600 RP-HPLC columns available to end users for purchase, some of which exhibit very large differences in selectivity and production quality. Often, two similar RP-HPLC columns are not equally suitable for the requisite separation, and to date, there is no universal RP-HPLC column covering a variety of analytes. This forces analytical laboratories to keep a multitude of diverse columns. Therefore, column selection is a crucial segment of RP-HPLC method development, especially since sample complexity is constantly increasing. Rationally choosing an appropriate column is complicated. In addition to the differences in the primary intermolecular interactions with analytes of the dispersive (London) type, individual columns can also exhibit a unique character owing to specific polar, hydrogen bond, and electron pair donor–acceptor interactions. They can also vary depending on the type of packing, amount and type of residual silanols, “end-capping”, bonding density of ligands, and pore size, among others. Consequently, the chromatographic performance of RP-HPLC systems is often considerably altered depending on the selected column. Although a wide spectrum of knowledge is available on this important subject, there is still a lack of a comprehensive review for an objective comparison and/or selection of chromatographic columns. We aim for this review to be a comprehensive, authoritative, critical, and easily readable monograph of the most relevant publications regarding column selection and characterization in RP-HPLC covering the past four decades. Future perspectives, which involve the integration of state-of-the-art molecular simulations (molecular dynamics or Monte Carlo) with minimal experiments, aimed at nearly “experiment-free” column selection methodology, are proposed.

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“…In-column modification of HPLC stationary phases is a useful technique due to the ease with which various bonded phases may be produced independent of parameters used to pack the sorbent [56,57]. While particulate media may be modified in batch mode before packing the column, functionalization using flow-through techniques is required for silica monoliths encased in polymer or prepared in capillaries in order to obtain the desired stationary phase displaying homogenous coverage of the support [22].…”

Section: Resultsmentioning

confidence: 99%

In‐column preparation of a brush‐type chiral stationary phase using click chemistry and a silica monolith

Slater

Fréchet

Švec³

2008

J of Separation Science

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Brush-type chiral stationary phases have been prepared both from a silica monolith and, separately, from 10 μm porous silica beads via a process of in-column modification including attachment of the chiral selector via copper catalyzed azide-alkyne cycloaddition. Azide functionalities were first introduced on the pore surface of each type of support by reaction with 3-(azidopropyl) trimethoxysilane, followed by immobilization of a proline-derived chiral selector containing an alkyne moiety. This functionalization reaction was carried out in dimethylformamide in the presence of catalytic amounts of copper(I) iodide. The separation performance of these triazole linked stationary phases was demonstrated in enantioseparations of four model analytes, which afforded separation factors as high as 11.4.

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On-column preparation of bonded phases for high pressure liquid chromatography

Cited by 34 publications

References 18 publications

In-situ chemically bonded stationary phases for high pressure liquid chromatography

In-situ chemically bonded stationary phases for high pressure liquid chromatography

Column Characterization and Selection Systems in Reversed-Phase High-Performance Liquid Chromatography

In‐column preparation of a brush‐type chiral stationary phase using click chemistry and a silica monolith

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