Chromatographic activity of residual silanols of alkylsilane derivatized silica surfaces

A.B. Scholten; H.A. Claessens; J.W. Haan, de; C.A.M.G. Cramers

doi:10.1016/S0021-9673(96)00765-0

Chromatographic activity of residual silanols of alkylsilane derivatized silica surfaces

A.B. Scholten, H.A. Claessens, J.W. Haan, de, C.A.M.G. Cramers

Chemical Engineering and Chemistry

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Abstract

Residual silanols on n-octadecylsilane derivatized silica surfaces have a pronounced effect on the chromatographic performance of reversed-phase high-performance liquid chromatography (RP-HPLC) materials. The present study describes how the results of solid-state NMR investigations on two commercially available reversed-phases for HPLC are verified chromatographically. One phase is a dimethyl-n-octadecylsilane derivatized silica substrate (Rx-C18), while the other is the same substrate derivatized with di-isobutyl-n-octadecylsilane ("stable bond", SB-C18). Four column tests, taken from the literature, are performed in order to assess silanol activity and column hyprophobicity. It is concluded that on the SB-C18 phase, more residual silanols are analyte accessible and that the isobutyl groups contribute significantly to hydrophobicity. Generally, the results of the solid-state NMR method for determining shielded and accessible residual surface silanols on RP-HPLC stationary phases could be confirmed.

Original language	English
Pages (from-to)	37-46
Journal	Journal of Chromatography, A
Volume	759
Issue number	1-2
DOIs	https://doi.org/10.1016/S0021-9673(96)00765-0
Publication status	Published - 1997

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title = "Chromatographic activity of residual silanols of alkylsilane derivatized silica surfaces",

abstract = "Residual silanols on n-octadecylsilane derivatized silica surfaces have a pronounced effect on the chromatographic performance of reversed-phase high-performance liquid chromatography (RP-HPLC) materials. The present study describes how the results of solid-state NMR investigations on two commercially available reversed-phases for HPLC are verified chromatographically. One phase is a dimethyl-n-octadecylsilane derivatized silica substrate (Rx-C18), while the other is the same substrate derivatized with di-isobutyl-n-octadecylsilane ({"}stable bond{"}, SB-C18). Four column tests, taken from the literature, are performed in order to assess silanol activity and column hyprophobicity. It is concluded that on the SB-C18 phase, more residual silanols are analyte accessible and that the isobutyl groups contribute significantly to hydrophobicity. Generally, the results of the solid-state NMR method for determining shielded and accessible residual surface silanols on RP-HPLC stationary phases could be confirmed.",

author = "A.B. Scholten and H.A. Claessens and \{Haan, de\}, J.W. and C.A.M.G. Cramers",

year = "1997",

doi = "10.1016/S0021-9673(96)00765-0",

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pages = "37--46",

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T1 - Chromatographic activity of residual silanols of alkylsilane derivatized silica surfaces

AU - Scholten, A.B.

AU - Claessens, H.A.

AU - Haan, de, J.W.

AU - Cramers, C.A.M.G.

PY - 1997

Y1 - 1997

N2 - Residual silanols on n-octadecylsilane derivatized silica surfaces have a pronounced effect on the chromatographic performance of reversed-phase high-performance liquid chromatography (RP-HPLC) materials. The present study describes how the results of solid-state NMR investigations on two commercially available reversed-phases for HPLC are verified chromatographically. One phase is a dimethyl-n-octadecylsilane derivatized silica substrate (Rx-C18), while the other is the same substrate derivatized with di-isobutyl-n-octadecylsilane ("stable bond", SB-C18). Four column tests, taken from the literature, are performed in order to assess silanol activity and column hyprophobicity. It is concluded that on the SB-C18 phase, more residual silanols are analyte accessible and that the isobutyl groups contribute significantly to hydrophobicity. Generally, the results of the solid-state NMR method for determining shielded and accessible residual surface silanols on RP-HPLC stationary phases could be confirmed.

AB - Residual silanols on n-octadecylsilane derivatized silica surfaces have a pronounced effect on the chromatographic performance of reversed-phase high-performance liquid chromatography (RP-HPLC) materials. The present study describes how the results of solid-state NMR investigations on two commercially available reversed-phases for HPLC are verified chromatographically. One phase is a dimethyl-n-octadecylsilane derivatized silica substrate (Rx-C18), while the other is the same substrate derivatized with di-isobutyl-n-octadecylsilane ("stable bond", SB-C18). Four column tests, taken from the literature, are performed in order to assess silanol activity and column hyprophobicity. It is concluded that on the SB-C18 phase, more residual silanols are analyte accessible and that the isobutyl groups contribute significantly to hydrophobicity. Generally, the results of the solid-state NMR method for determining shielded and accessible residual surface silanols on RP-HPLC stationary phases could be confirmed.

U2 - 10.1016/S0021-9673(96)00765-0

DO - 10.1016/S0021-9673(96)00765-0

M3 - Article

SN - 0021-9673

VL - 759

SP - 37

EP - 46

JO - Journal of Chromatography, A

JF - Journal of Chromatography, A

IS - 1-2

ER -

Chromatographic activity of residual silanols of alkylsilane derivatized silica surfaces

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