High-endurance packing material for liquid chromatography
View Patent ↗The present invention provides a highly durable packing material for liquid chromatography that is excellent in acidic resistance and alkalic resistance. Such a packing material for liquid chromatography can be obtained by chemically modifying silica gel with a bifunctional silane compound represented by the general formula [I], and carrying out an endcapping reaction of the resulting chemically modified silica gel using bifunctional cyclic silazane represented by the general formula [II]. In the formula [I], X 1 and X 2 , the same or different, represent a hydrogen atom, a halogen atom or an alkoxy group having 1 to 4 carbon atoms; and R 1 represents an alkyl group or an aryl group, which can have substituent(s). In the formula [II], R 2 and R 3 , the same or different, represent an alkyl group having 1 to 4 carbon atoms; and n represents a value indicating unit number that forms the ring, which is an integer of 2 to 10.
1. A method of the production of a packing material for liquid chromatography which comprises chemically modifying silica gel with a bifunctional silane compound represented by the general formula [I]:
[wherein, X 1 and X 2 , the same or different, represent a hydrogen atom, a halogen atom or an alkoxy group having 1 to 4 carbon atoms; and R 1 represents an alkyl group or an aryl group which can have substituent(s)], and
carrying out an endcapping reaction of the resulting chemically modified silica gel using bifunctional cyclic silazane represented by the general formula [II]:
[wherein, R 2 and R 3 , the same or different, represent an alkyl group having 1 to 4 carbon atoms; and n represents a value indicating unit number that forms the ring, which is an integer of 2 to 10].
2. The method of the production of a packing material for liquid chromatography according to claim 1 wherein the alkyl group represented by R 1 in the general formula [I] has an aryl group, an amino group, a cyano group or a nitro group at the end thereof, or has an amide group, a carbamate group, a carbamide group, an ester group or a carbonate group at a site other than the end thereof.
3. The method of the production of a packing material for liquid chromatography according to claim 1 or 2 wherein bifunctional cyclic silazane represented by the general formula [II] and a bifunctional silane compound represented by the general formula [III]:
[wherein, X 3 and X 4 , the same or different, represent a hydrogen atom, a halogen atom or an alkoxyl group having 1 to 4 carbon atoms; and R 4 and R 5 , the same or different, represent an alkyl group having 1 to 4 carbon atoms] are used in combination.