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Polar-modified bonded phase materials for chromatographic separations

  • US 7,125,488 B2
  • Filed: 02/12/2004
  • Issued: 10/24/2006
  • Est. Priority Date: 02/12/2004
  • Status: Active Grant
First Claim
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1. A composition for use as a stationary phase in chromatography comprising an inorganic substrate that is modified with at least one silane having the formula
R1δ

  • -Qα

    -(CH2)β

    SiR2γ

    X3-γ

    ,wherein R1 is hydrogen, C1

    C100 substituted or unsubstituted hydrocarbyl, cycloalkyl, heterocycloalkyl, aryl, or heteroaryl;

    wherein the substituents are selected from C1

    C12 hydrocarbyl, hydroxyl, alkoxy, halogen, amino, nitro, sulfo, and carbonyl;

    α

    is 0 or 1;

    β

    is 0–

    30;

    γ

    is 0, 1 or 2;

    δ

    is 0–

    3;

    R2 is C1

    C100 substituted or unsubstituted hydrocarbyl, cycloalkyl, heterocycloalkyl, aryl, or heteroaryl;

    wherein the substituents are selected from C1

    C12 hydrocarbyl, hydroxyl, alkoxy, halogen, amino, nitro, sulfo, and carbonyl;

    Q is independently selected from —

    NHC(O)—

    , —

    C(O)NH—

    , —

    OC(O)NH—

    , —

    NHC(O)O—

    , —

    NHC(O)NH—

    , —

    NCO, —

    CHOHCHOH—

    , CH2OCHCH2O—

    , —

    (CH2CH2O)n

    , —

    (CH2CH2CH2O)n

    , —

    C(O)—

    , —

    C(O)O—

    , —

    OC(O)—

    , CH3C(O)CH2

    , —

    S—

    , —

    SS—

    , —

    CHOH—

    , —

    O—

    , —

    SO—

    , —

    SO2

    , —

    SO3

    , —

    OSO3

    , —

    SO2NH—

    , —

    SO2NMe—

    , —

    NH—

    , —

    NMe—

    , —

    NMe2+

    , —

    N[(CH2)n]2+

    , —

    CN, —

    NC, —

    CHOCH—

    , —

    NHC(NH)NH—

    , —

    NO2, —

    NO, —

    OPO3

    , where n is 1–

    30; and

    X is a leaving group.wherein said inorganic substrate is equilibrated in an atmosphere having a defined relative humidity of less than 40% prior to being modified with the at least one silane, sufficiently to minimize anion exchange activity and enhance stability to base and acid treatment.

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