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Nitro-benzene boric-acid affinity chromatographic pre-column, its production and use

A technology for nitrating phenylboronic acid and nitrating phenylboron, which is applied in chemical instruments and methods, other chemical processes, chemical/physical processes, etc., can solve problems affecting sample stability, column bed is not dense and stable, and quantitative deviation is large, and achieves Good qualitative and quantitative results, increased affinity and prolonged stability

Inactive Publication Date: 2007-04-04
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

The applicant had previously used the commercial phenylboronic acid affinity gel Affi-Gel601 purchased from Bio-Rad, which uses acrylamide as a support for the affinity of nucleosides in urine samples in a classical glass column with a larger diameter Pretreatment is cumbersome, and the material is often deformed when it swells in the column, so the packed column bed is not dense and stable, which will affect the stability of parallel processing of samples, resulting in large quantitative deviations

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  • Nitro-benzene boric-acid affinity chromatographic pre-column, its production and use
  • Nitro-benzene boric-acid affinity chromatographic pre-column, its production and use
  • Nitro-benzene boric-acid affinity chromatographic pre-column, its production and use

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Embodiment 1

[0029] Among the drugs used, m-aminophenylboronic acid, LiChrosorb Si100, 5 μm silica gel and γ-glycidyloxypropyltrimethoxysilane were purchased from Sigma, and the rest were of analytical grade.

[0030] (1) Synthesis of Silica-Based Phenylboronic Acid Filler

[0031] Preparation of functional group nitrated phenylboronic acid: Weigh 1.1160 g of m-aminophenylboronic acid, dissolve in 24 ml of twice distilled water, add 0.80 ml of benzoyl chloride, and shake for 1 hour under nitrogen protection. Ethyl acetate was extracted three times, 30ml each time, the organic layers were combined, and vacuum-dried. The product was added to 5ml H in an ice bath 2 SO 4 / HNO 3 (4:1, v / v) mixed acid, after dissolving, add saturated sodium hydroxide and sodium bicarbonate solution to pH 3.0, ice bath, and slowly add dropwise. Add an equal volume of ethyl acetate for three extractions, combine the organic layers, and vacuum dry. The product was passed through a silica gel column with ethano...

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Abstract

A nitrated phenylboric acid affinity chromatographic pre-column for in-line collecting the cis-dihydroxy compounds in HPLC features that its filler is the silicon gel based nitrated phenylboric acid. It is suitable for the in-line analysis system of HPLC by use of parallel two pre-columns to obtain high qualitative and quantitative correctness. Its preparing process is also disclosed.

Description

technical field [0001] The invention relates to an affinity chromatographic column, in particular to a nitrophenylboronic acid affinity chromatographic pre-column and its preparation and application. Background technique [0002] Affinity chromatography is a powerful tool for the separation and analysis of various biomolecules, and boronic acid affinity chromatography is one of the most important types. Under alkaline conditions, the boronic acid group can interact with the Linshun dihydroxyl structure to form a stable five-membered ring complex, and the complex is opened under acidic conditions. This feature endows boric acid affinity chromatography materials with the ability to enrich and extract various biomolecules containing adjacent dihydroxy structures, among which boric acid affinity chromatography materials with phenylboronic acid as the functional group are most widely used, and the reported enrichment, Purification and separation are widely used, such as the sepa...

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Application Information

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IPC IPC(8): B01D15/08B01J20/22
Inventor 许国旺李方楼赵欣捷
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI