Amphoteric electrolyte-modified hybrid silica gel material and solid-phase extraction method thereof
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A technology of amphoteric electrolyte and hybrid silica gel, which is applied in organic chemical methods, chemical instruments and methods, amphoteric ion exchange, etc., to achieve fast adsorption and desorption, good reproducibility, and high recovery rate
Inactive Publication Date: 2015-06-03
NINGBO UNIVERSITY OF TECHNOLOGY
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[0005] At present, the composite adsorption mechanism of solid phase extraction is only a combination of reverse phase and anion (cation) ion exchange, and does not combine the cation exchange mechanism and anion exchange mechanism on the same stationary phase to achieve the extraction of acidic, neutral and alkaline samples.
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Embodiment 1
[0028] The synthetic route for the preparation of hybrid silica gel modified by ampholyte is as follows figure 1 As shown, tetraethoxysilane (TEOS) and aminopropyltriethoxysilane (APTES) are precursor molecules, cetyltrimethylammonium bromide (CTAB) is used as template, and absolute ethanol As the solvent, a hybrid silica gel material containing amine groups on the surface was prepared by the sol-gel method ( figure 1 ). The amine group of the hybrid silica gel material reacts with the excess aldehyde group of glutaraldehyde under the condition of pH 8.0 to generate C=N, so that the surface of the hybrid silica gel is bonded to the aldehyde group. The same method is used. Under the condition of pH 8.0, the aldehyde group at the other end of the glutaraldehyde bonded to the hybrid silica gel reacts with the amine group of the excessive amphoteric electrolyte to produce C=N, which is unstable, so NaCNBH is required 3 Reduce C=N to stable C-N ( figure 1 ).
[0029] The specific synt...
Embodiment 2
[0032] Weigh 50 mg of the hybrid silica gel material modified with amphoteric electrolyte prepared in Example 1, and put it into a 3mL column tube with a 5μm aperture lower sieve plate, fill it with a 20μm aperture upper sieve plate, and shake it evenly with a vibrating bed. Machine compaction.
Embodiment 3
[0034] The quartz capillary passes through the concentrated HNO 3 (10min), distilled water, HF (10min), distilled water, 1mol / L NaOH (12h), distilled water, 0.1mol / L HCl (1h), distilled water, methanol after treatment, put the quartz capillary column in the gas chromatography furnace, N at 120°C 2 Dry under flow for 3h, and mix 112μL tetraethoxysilane (TEOS), 118μL aminopropyltriethoxysilane (APTES), 215μL absolute ethanol, 32μL water and 8mg cetyltrimethylammonium bromide (CTAB) After mixing thoroughly, introduce the pretreated quartz capillary through a syringe, seal both ends with silicone rubber, and heat 40℃ to react and polymerize for 24 h. The polymerized material is flushed with ethanol through a constant flow syringe pump to remove CTAB (30min ), rinse with water and 100mmol / L phosphate (pH 8.0), and then continuously pump in 100mmol / L phosphate (pH 8.0) containing 10% glutaraldehyde, react at 90℃ for 0.5h, rinse with phosphate buffer 30min, add 31μL 10% ampholyte and ...
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Abstract
The invention discloses an amphoteric electrolyte-modified hybrid silica gel material. An amphoteric electrolyte containing an amino group and a carboxyl group is bonded on a branch of the hybrid silica gel to obtain a hybrid silica gel material with an amphoteric group on the surface. A preparation method of the hybrid silica gel material comprises the following steps of: forming a hybrid silica gel material containing amino on the surface by taking tetraethoxy silane and aminopropyltriethoxy silane as precursor molecules and taking hexadecyl trimethyl ammonium bromide as a template agent; enabling the hybrid silica gel to react with the aldehyde group of glutaraldehyde to generate a hybrid silica gel material with a C=N bond; enabling the aldehyde group at the other end of glutaraldehyde on the hybrid silica gel material to react with the amphoteric electrolyte with the amino group and the carboxyl group to generate a hybrid silica gel material with double C=N bonds; and reducing with NaCNBH3 to reduce C=N into C-N to form a hybrid silica gel material with multiple -NH2 groups and multiple -COOH groups. A solid-phase extraction column or solid-phase extraction capillary tube prepared from the hybrid silica gel material gives play to the advantages of anion-cation exchange on the same material at the same time by controlling the pH value, and realizes synchronous extraction of acid, neutral and alkali samples; and moreover, the adsorption and desorption are fast, the reproducibility and recovery rate are high, and the speed and precision of detection and separation can be improved.
Description
Technical field [0001] The invention relates to the technical field of sample pretreatment, in particular to a hybrid silica gel material modified with an amphoteric electrolyte and a solid phase extraction method thereof. Background technique [0002] Solid phase extraction technology (SPE) is the use of selective adsorption and selective elution to enrich, separate and purify samples, including physical extraction processes of liquid and solid phases. It is not only suitable for extracting and enriching food and environmental water Trace organic compounds in the sample, and suitable for the enrichment of the measured components in biological samples. [0003] The main representatives of the composite adsorption mechanism of solid-phase extraction materials are Oasis MCX and Oasis WCX. Their adsorption mechanism combines reverse phase retention and strong (weak) cation exchange, which is limited to the analysis of basic samples, or Oasis MAX and Oasis WAX. Combined with reversed-...
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