Hydrophilic interaction chromatography/ ion exchange chromatography mixed stationary phase and preparation and application thereof

A technology of ion exchange chromatography and mixed stationary phase, which is applied in the direction of ion exchange, cation exchange, anion exchange, etc., can solve the problems of easy hydrolysis, short column life, easy oxidation, etc., and achieve strong separation ability, small column pressure and stable structure Effect

Active Publication Date: 2017-04-05
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] As a widely used commercial amino column at present, it shows excellent separation ability for the separation of polar compounds, but it is easy to oxidize and hydrolyze during use, resulting in short column life

Method used

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  • Hydrophilic interaction chromatography/ ion exchange chromatography mixed stationary phase and preparation and application thereof
  • Hydrophilic interaction chromatography/ ion exchange chromatography mixed stationary phase and preparation and application thereof
  • Hydrophilic interaction chromatography/ ion exchange chromatography mixed stationary phase and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Weigh 4.393g of silica gel and place it in a 100mL three-necked flask, add 40mL of anhydrous toluene, 6.418g of 3-chloropropyltrimethoxysilane, and 80 μL of triethylamine as a catalyst through a dropping funnel. Under the protection of argon, the reaction was refluxed for 24 hours. After the reaction was completed, it was filtered, the bonded silica gel was extracted with acetone for 24 hours, and 4.913 g of silanized silica gel was obtained after drying.

[0037] Weigh 4.127g of imidazole and 10.013g of anhydrous potassium carbonate in a 250mL three-neck flask, add 50mL of acetone with the dropping funnel, add 3-chloropropylamine hydrochloride dissolved in 50mL of acetone with the dropping funnel under stirring, then add 50mL of acetone , Under the protection of argon, the reaction was refluxed for 6hr. After the reaction is finished, filter, remove the acetone by rotating the filtrate with a water pump under reduced pressure, and then use an oil pump to distill the p...

Embodiment 2

[0044] The chromatographic column obtained above was used to separate monosaccharides, disaccharides and trisaccharides under the mode of hydrophilic interaction chromatography. High performance liquid chromatography differential refraction detection method was used, with acetonitrile / water (85 / 15, v / v) as the mobile phase, isocratic elution, the flow rate was 1.0 mL / min, and the detection temperature was 30°C. Chromatograms such as figure 2 As shown (1 is rhamnose, 2 is xylose, 3 is fructose, 4 is mannose, 5 is glucose, 6 is sucrose, 7 is maltose, 8 is lactose, 9 is trehalose, 10 is melibiose, 11 is raffinose, 12 is melezitose).

[0045] Depend on figure 2 It can be seen that the chromatographic column of the present invention can completely separate 12 kinds of carbohydrate compounds at one time, showing excellent separation ability.

Embodiment 3

[0047] Using the chromatographic column (a) prepared in the above examples, commercialized classic amino column (Fuji amino silica gel filler) (b), Waters high-efficiency carbohydrate analysis column (classic silica gel amino column) (c) in the hydrophilic interaction chromatography mode Separation of sugar compounds. High performance liquid chromatography differential refraction detection method was used, with acetonitrile / water (85 / 15, v / v) as the mobile phase, isocratic elution, the flow rate was 1.0 mL / min, and the detection temperature was 30°C. Chromatograms such as image 3 As shown (1 is rhamnose, 2 is xylose, 3 is fructose, 4 is mannose, 5 is glucose, 6 is sucrose, 7 is maltose, 8 is trehalose).

[0048] Depend on image 3 It can be seen that the chromatographic column of the present invention has a stronger retention capacity for sugar compounds than the other two classic amino columns.

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Abstract

The invention relates to high-performance liquid chromatography stationary phases, in particular to a hydrophilic interaction chromatography/ ion exchange chromatography mixed stationary phase and preparation and application of the hydrophilic interaction chromatography/ ion exchange chromatography mixed stationary phase. The structure of the hydrophilic interaction chromatography/ ion exchange chromatography mixed stationary phase is shown as the formula 1, and please see the formula 1 in the specifications, wherein X is -OCH3 or -OCH2CH3, Y1 is F or Cl or Br or I or BF4 or Tf2N or CF3SO3 or SCN or NO2 or NO3, Y2 is -NHCH3 or -N (CH3)2 or -N+ (CH3)3Y1 or -NHCH2CH3 or -N (CH2CH3)2 or -N+ (CH2CH3)3Y1, and n=2 or 3. According to the prepared mixed type stationary phase, raw materials are easy to obtain and the preparation procedure are simple; and the prepared mixed type stationary phase has good retaining performance and separation selectivity for multiple saccharides and has good application and popularization prospects.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography stationary phase, in particular to a hydrophilic interaction chromatography / ion exchange chromatography mixed stationary phase and its preparation and application. Background technique [0002] High performance liquid chromatography (HPLC) is a rapid and sensitive chromatographic technique developed in the 1960s, widely used in small molecules [Ding X., Wang X., Chen L., et al. Analysis and separation in various fields such as J. Chromatogr.A, 2011, 1218, 1227.] and macromolecules [Wattanasiritham L., Theerakulkait C., Maier C. Food Chem, 2016, 192, 156.]. Among them, reversed-phase liquid chromatography (RPLC) is currently the most widely used high-efficiency separation technology, but the hydrophobic stationary phase (such as C18, C8, etc.) Polar oligopeptides, etc.) have weak or even no retention, so strongly polar compounds cannot be well separated on RPLC. Hydrophilic interaction ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30B01D15/36B01D15/32C13K1/04C13K1/08C13K7/00C13K13/00C07H3/02C07H3/04C07H3/06C07H1/06
CPCB01D15/32B01D15/361B01J20/286B01J2220/52C07H1/06C07H3/02C07H3/04C07H3/06C13B20/126C13K1/04C13K1/08C13K7/00C13K13/002
Inventor 黄少华杨晨曦杨海燕高峻
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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