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Mixed fillers of liquid-phase chromatographic column and chromatographic column

A technology of liquid chromatography column and mixed packing, applied in the field of liquid chromatography column mixed packing and chromatography column, can solve the problems of excessive retention, low detection efficiency, decreased signal sensitivity, etc., and achieves simple method and good reproducibility Effect

Active Publication Date: 2012-04-18
天津博纳艾杰尔科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Octadecyl bonded silica gel is the most commonly used reversed-phase liquid chromatography column packing. This type of column has high column efficiency, long life and wide application range. However, the main disadvantage of this column is that it is extremely hydrophilic for some Some compounds are too weakly retained to be separated, and some lipophilic compounds are too strongly retained to be eluted
When a sample contains both highly hydrophilic and lipophilic compounds, it is difficult to complete the analysis and detection of all components of the sample through a single liquid chromatography separation, and it is even more difficult when using isocratic liquid chromatography separation mode. difficult to achieve
Taking a sample containing both hydrophilic substances such as uracil and lipophilic polycyclic aromatic hydrocarbons as an example, when octadecyl-bonded silica gel (C18) is used for reversed-phase chromatography separation, the retention of hydrophilic substances is too weak to be separated , while the retention of PAHs is too strong, it takes a long time to elute, not only the signal sensitivity decreases, which affects the accuracy, but also the detection efficiency is too low

Method used

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  • Mixed fillers of liquid-phase chromatographic column and chromatographic column
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  • Mixed fillers of liquid-phase chromatographic column and chromatographic column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Silica gel preparation

[0037] Add 1240ml of purified water, 26g of concentrated nitric acid, 840g of silica sol (7.1%) and 37g of urea into a 6000ml beaker in sequence, and stir until the urea dissolves.

[0038] Add 100g of formaldehyde under rapid stirring, continue stirring for 15 seconds, room temperature 25°C.

[0039] After standing for 10-15min, a white precipitate precipitated out.

[0040] Stand for 5-8 hours, skim off the upper liquid, add pure water to stir, let stand for 30 minutes, skim off the upper liquid.

[0041] Wash 3 times with acetone and filter. Vacuum at 100°C and dry for 12 hours. Microscopic examination showed 4--5μm, spherical and uniform.

[0042] High temperature firing, 300°C, 3-4h; 500°C, 2-3h; 800°C, 2h; 1000°C, 3h.

[0043] After burning, 53 g of white solid was obtained; heated to 90° C. in 400 ml of 0.5 M HF aqueous solution for 4 hours; filtered, washed twice with 200 ml of pure water and three times with 200 ml of acetone; drie...

example 1

[0045] Add 50 g of silica gel prepared in Example 1, add 4 g of tetraethoxysilane, 1 g of triethylamine, and 200 ml of toluene; heat under electric stirring at 110 ° C for 16 hours; filter, wash with toluene 3 times, each dose of 100 ml, and Wash 3 times with methanol, each dose 100ml, then stir and wash with methanol and water mixture 3 times, each dose 150ml, wherein the volume ratio of methanol to water is 1:1, then wash 3 times with methanol, each dose 100ml; vacuum-dried at 100°C for 12 hours; 52g of white spherical solid powder was obtained. C % = 0.2.

example 2

[0047] The white solid 20g that prepares in the example 2, add EtOSi (CH 3 ) 2 CH 2 CH 2 CONH 2 10g, triethylamine 1g, toluene 100ml; heated at 110°C for 18 hours under electric stirring; filtered, washed 3 times with toluene, each dose 100ml, then washed 3 times with methanol, each dose 100ml, then methanol and water The mixed solution was stirred and washed 3 times, each dosage 150ml, wherein the volume ratio of methanol to water was 1:1, and then washed 3 times with methanol, each dosage 100ml; vacuum dried at 100°C for 10 hours; white spherical solid powder was obtained 22g. C% = 3.2, N% = 0.8. (0.5mmol / g)

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Abstract

The invention relates to mixed fillers of a liquid-phase chromatographic column and the chromatographic column, and relates to the technical field of analytical chemistry. The mixed fillers of the liquid-phase chromatographic column comprise long-chain alkyl dimethyl silane bonded silica gel and acylamino silane bonded silica gel in a weight ratio of 10:1-1:10, wherein the difference of the mean particle diameter is in a range of between -20 and 20 percent and the difference of the specific weight is in a range of between -20 and 20 percent. In the chromatographic column made by the mixed fillers, the mixed fillers are filled in a column pipe; the outer sides of the two ends of the column pipe are connected with a pipeline through internal thread; the inner sides of the two ends of the column pipe are provided with sieve plates used for preventing the mixed fillers from leaking outwards; one end of the column pipe is provided with a liquid inlet; and a mobile phase enters the chromatographic column from the liquid inlet. The characteristics of the mixed fillers of the liquid-phase chromatographic column are applied to chromatographic separation under the condition of the mixed mobile phase containing acetonitrile and aqueous solution, wherein the separation application is the chromatographic separation and detection of a sample containing a compound with extremely strong hydrophilism and a compound with extremely strong lipotropism simultaneously; and the separation detection of all the components can be performed once under the condition of equal-grade liquid-phase chromatogram.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a liquid phase chromatographic column mixed filler and a chromatographic column. Background technique [0002] Liquid chromatography is a widely used analytical chromatographic technique. The basic principle is that the components with strong affinity with the stationary phase in the sample stay in the stationary phase for a long time, while the components with weak affinity with the stationary phase flow out quickly. stationary phase for the purpose of separation. [0003] Octadecyl bonded silica gel is the most commonly used reversed-phase liquid chromatography column packing. This type of column has high column efficiency, long life and wide application range. However, the main disadvantage of this column is that it is extremely hydrophilic for some Some compounds are too weakly retained to be separated, and some lipophilic compounds are too strongly retained to ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/281B01D15/08
Inventor 朱旭东王宛
Owner 天津博纳艾杰尔科技有限公司
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