Mixed-mode chromatography stationary phase based on hydrophobic effect and silver ion pi effect and preparation method and use thereof

A technology of mixed-mode chromatography and complexation, which is applied in the field of preparation of mixed-mode chromatography stationary phases, can solve the problems of unfavorable high-efficiency and rapid analysis, cumbersome operation, environmental pollution, etc., and achieve good selection of separation ability, separation effect, heavy good effect

Inactive Publication Date: 2013-01-30
INST OF OIL CROPS RES CHINESE ACAD OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the offline mode needs to collect the first-dimensional fraction first, concentrate and other treatments, and then perform the second-dimensional separation. The operation is cumbersome and time-consuming, which is not conducive to high-throughput analysis, but also easily leads to high costs and environmental pollution.
Although the online mode has the advantages of a high degree of automation, the complexity of the system increases, and the dead volume caused by the conversion valve, loop line, etc. increases the risk of peak broadening; and for the separation mode of two different retention mechanisms, two-dimensional solvents must also be considered. compatibility, which is very unfavorable for efficient and fast analysis

Method used

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  • Mixed-mode chromatography stationary phase based on hydrophobic effect and silver ion pi effect and preparation method and use thereof
  • Mixed-mode chromatography stationary phase based on hydrophobic effect and silver ion pi effect and preparation method and use thereof
  • Mixed-mode chromatography stationary phase based on hydrophobic effect and silver ion pi effect and preparation method and use thereof

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Experimental program
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Effect test

Embodiment 1

[0039] Embodiment 1: a kind of preparation method of the mixed-mode chromatographic stationary phase based on hydrophobic interaction and silver ion π complexation, it comprises the steps:

[0040] 1) Preparation of octyl-mercapto bonded silica gel: Take 3.0 g of vacuum-dried silica gel (silica gel microspheres for chromatography, with a particle size of 5 μm) in a 250 mL three-necked flask, add 120 mL of treated anhydrous toluene, 1.28 g 3-mercaptopropyltriethoxysilane and 1.50g octyltriethoxysilane, stir mechanically, add 3 drops of triethylamine (about 0.9mL) dropwise, heat under N2 protection and reflux for 30h, cool, pump Filter, wash with toluene, methanol and acetone successively; After vacuum drying at 70°C for 5h (vacuum degree is -50KPa), octyl-mercapto bonded silica gel is obtained, which is ready for use.

[0041] 2). Preparation of hydrophobic / strong cation exchange mixed mode silica gel stationary phase (octyl-sulfonate bonded silica gel): Take 3.0g of octyl-merc...

Embodiment 2

[0049] Embodiment 2: a kind of preparation method of the mixed-mode chromatographic stationary phase based on hydrophobic interaction and silver ion π complexation, it comprises the steps:

[0050] 1). Preparation of octyl-mercapto bonded silica gel: Take 3.0g of vacuum-dried silica gel in a 250mL three-neck flask, add 120mL of treated anhydrous toluene, 1.28g of 3-mercaptopropyltriethoxysilane and 1.50 g of octyltriethoxysilane, mechanically stirred, and 3 drops of triethylamine (0.9 mL) were added dropwise. N 2 After heating under reflux for 30 h under protection, cool, filter with suction, and wash with toluene, methanol and acetone in turn. After vacuum drying at 70°C for 5h (vacuum degree is -30KPa), an octyl-mercapto bonded silica gel was obtained, which is ready for use.

[0051] 2). Preparation of hydrophobic / strong cation exchange mixed mode silica gel stationary phase (octyl-sulfonate bonded silica gel): Take 3.0g of octyl-mercapto bonded silica gel in a 100mL thre...

Embodiment 3

[0060] A preparation method of a mixed-mode chromatographic stationary phase based on hydrophobic interaction and silver ion π complexation, which comprises the following steps: 1) first preparing a hydrophobic / strong cation exchange mixed-mode silica gel stationary phase, and then making a columnar Hydrophobic / strong cation exchange mixed-mode silica gel stationary phase;

[0061] ①Using 120mL of anhydrous toluene as an organic solvent, add 3g of silica gel and 1g of silane coupling agent (0.5g 3-mercaptopropyltrimethoxysilane, 0.5g octyltrimethoxysilane), mechanically stir, drop into (2 drops, about 0.6mL) triethylamine as catalyst, in N 2 After heating and reflux reaction under protection for 20 hours, cooling, suction filtration, washing with toluene, methanol, acetone successively; Mercapto-bonded silica gel;

[0062] 2. Add methanol and hydrogen peroxide solution with a concentration of 25wt% to the octyl-mercapto bonded silica gel prepared in step 1. The volume ratio ...

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Abstract

The invention relates to chromatography stationary phase material and a preparation method and use thereof. Mixed-mode chromatography stationary phase based on hydrophobic effect and silver ion pi effect is characterized in that according to a structural formula, R is methoxyl, ethyoxyl or Cl; the mixed-mode chromatography stationary phase is characterized by simple preparation and good separation effect; the mixed-mode chromatography stationary phase is used for separating triglyceride from grease; separation effect is good; in addition, the mixed-mode chromatography stationary phase has good application prospect.

Description

technical field [0001] The invention relates to a chromatographic solid-phase material and a preparation method thereof, in particular to a preparation method of a mixed-mode chromatographic stationary phase based on hydrophobic interaction and silver ion π complexation. Background technique [0002] Triacylglycerols (TAGs) is the main component of vegetable oil (accounting for more than 95%). It is formed by the condensation of one glycerol molecule and three fatty acid molecules. The carbon chain length of the fatty acid, the position of the fatty acid on the glycerol skeleton (sn-1, sn-2 and sn-3 positions from top to bottom), and the number of double bonds (DBs) of the fatty acid have an important influence on the properties of vegetable oil. Since natural oils and fats have unique triglyceride composition, it is expected to efficiently and accurately identify various edible vegetable oils and adulterated vegetable oils through efficient and highly sensitive qualitative ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30B01D15/08A23D9/00
Inventor 魏芳冯钰锜籍淑贤董绪燕陈洪胡娜吕昕
Owner INST OF OIL CROPS RES CHINESE ACAD OF AGRI SCI
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