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Polyvinyl alcohol coating chromatography stationary phase as well as preparation method thereof and application

A chromatographic stationary phase and polyvinyl alcohol technology, which is applied in the field of polyvinyl alcohol-coated chromatographic stationary phases, can solve the problems of affecting the reproducibility of analysis results, the complex preparation process of the stationary phase, and the limited range of pH application, and achieve the design idea. Novel, technically applicable, good retention and effect of separation properties

Inactive Publication Date: 2014-12-24
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation process of the stationary phase is complex and extremely time-consuming
It should be pointed out that bare silica itself can be used as a HILIC stationary phase, but its main defect is that the applicable range of pH is limited, and the reaction of residual silanol on the surface can easily lead to some irreversible adsorption, which affects the reproducibility of analytical results.

Method used

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  • Polyvinyl alcohol coating chromatography stationary phase as well as preparation method thereof and application
  • Polyvinyl alcohol coating chromatography stationary phase as well as preparation method thereof and application
  • Polyvinyl alcohol coating chromatography stationary phase as well as preparation method thereof and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Weigh 1g of polyvinyl alcohol (PVA), add it into a 100mL round-bottomed flask to prepare a PVA aqueous solution with a concentration of 0.02g / mL, stir at 100°C and 1500rpm until the PVA is evenly dissolved, then add 3g of silica gel, and continue stirring at 300rpm for 20min , filter while hot with a sand core funnel, wash the solid product with water, put it in an oven and dry it at 140°C to obtain the stationary phase.

[0034] The obtained stationary phase filler was filled in a 4.6mm*150mm, I.D. stainless steel HPLC chromatographic column, and the prepared chromatographic column was used to test its retention and separation of strongly polar compounds in the hydrophilic chromatography mode and to separate mixed samples. The mobile phase is three phases, which are respectively acetonitrile, water, and 250 mM ammonium formate solution (pH is 3.51). The mobile phase conditions are that the volume ratio of acetonitrile, water and ammonium formate is 90 / 4 / 6, the flow rat...

Embodiment 2

[0036] The difference from Example 1 is that according to the synthesis steps of Example 1, the filtered solid product is first put into a refrigerator at -20°C and frozen to obtain a cold-polymerized polyvinyl alcohol stationary phase.

[0037] The chromatographic column obtained by packing the obtained stationary phase was used to separate samples in normal phase chromatography mode. The mobile phase condition was that the volume ratio of n-hexane and ethanol was 80 / 20. Four kinds of samples have been well separated, and the chromatogram is as shown in 2 (1 is phenol, 2 is o-diphenol, 3 is m-diphenol, 4 is 4-nitroaniline); Equally, prepared chromatographic column is in Separation of cephalosporin samples in hydrophilic interaction chromatography mode. Using acetonitrile, water, 250mM ammonium formate solution (pH 5.7) as the mobile phase, and gradient elution (water volume content: 0-60 minutes: 10-40%), the cephalosporin samples are well retained and separated , the chrom...

Embodiment 3

[0039] The difference from Example 2 is that sodium dodecyl sulfate (SDS) is added in the polyvinyl alcohol solution, and the chromatographic column packed with another polyvinyl alcohol stationary phase and this stationary phase can be obtained according to the synthetic steps of Example 1 . The sodium dodecyl sulfate (SDS) structural formula of this implementation is:

[0040]

[0041] The prepared chromatographic column was used to separate polycyclic aromatic hydrocarbon samples under the mode of reverse phase chromatography. The mobile phase conditions were methanol and water at a volume ratio of 20 / 80. The chromatogram is shown in 4 (1 is uracil, 2 is benzene, 3 is toluene, 4 is naphthalene, 5 is biphenyl, 6 is phenanthrene, 7 is pyrene).

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Abstract

The invention discloses a polyvinyl alcohol coating chromatography stationary phase as well as a preparation method and application thereof. The preparation method comprises the following steps: a, preparing a polyvinyl alcohol aqueous solution; b, coating the surface of each spherical particle, namely, adding the spherical particles into the polyvinyl alcohol aqueous solution obtained in the step a, stirring the spherical articles at 300 to 1500rpm so as to uniformly mix the spherical articles and the aqueous solution; and c, washing and drying, namely, filtering a reaction system in the step b, washing a solid product by utilizing water, and performing vacuum drying on the solid product to be used as packing stuffing. The polyvinyl alcohol coating chromatography stationary phase and the preparation method have the advantages that the coating-type material is prepared by utilizing a physical coating principle, and the design concept is novel and environment-friendly. The coating process is completed in the aqueous solution system, the operation process is simple and convenient, and the reaction condition is moderate. The technology of the preparation method is wide in application range, a compound of the needed functional group is added in the polyvinyl alcohol aqueous solution to perform the coating, the stationary phase of any function can be prepared, and a wide development space is provided for the polyvinyl alcohol immobilization stationary phase.

Description

technical field [0001] The invention relates to the field of hydrophilic chromatographic stationary phases, in particular to a polyvinyl alcohol-coated chromatographic stationary phase. Background technique [0002] Hydrophilic interaction chromatography (HILIC) was first proposed by Alpert in 1990. Its basic feature is that it adopts a stationary phase similar to normal phase chromatography, and uses a mobile phase similar to reversed phase chromatography. It can effectively solve the shortcomings of reversed-phase chromatography that cannot effectively separate highly polar compounds, and at the same time overcome the defect of low solubility of polar compounds in normal phase chromatography mode, and is widely used for the separation of highly polar compounds. In addition, its high proportion of organic phase makes it compatible with mass spectrometry, which improves the detection sensitivity of separation and analysis. [0003] As a key component of hydrophilic interac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/281B01J20/26B01J20/30B01D15/08
Inventor 章飞芳杨丙成纪顺利沈国滨何成霞汪媛朱银芳
Owner EAST CHINA UNIV OF SCI & TECH
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