Preparing method of capillary tube chromatographic columns

A technology of capillary chromatographic column and capillary column, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of low preparation success rate, complicated preparation process of capillary chromatographic column, long preparation cycle, etc., and achieve the effect of simple and fast method

Inactive Publication Date: 2012-07-18
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims to provide a fast, simple, high-throughput parallel preparation method for capillary chromatographic columns for the problems of complex preparation process, long preparation period, and low preparation success rate of capillary chromatographic columns.

Method used

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  • Preparing method of capillary tube chromatographic columns
  • Preparing method of capillary tube chromatographic columns

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Preparation of C18 reversed-phase capillary column

[0027] 1. Preparation of homogenate

[0028] Weigh 50 mg of C18 reversed-phase silica gel bonded stationary phase with a particle size of 3 μm, add the obtained filler into 10 ml of acetone to prepare a homogenate with a concentration of 5 mg / ml, and shake the solution by hand to mix it evenly, and then Oscillate in an oscillator for 10 minutes to evenly distribute the filler in acetone.

[0029] 2. Prepare the outlet plunger

[0030] Cut 8 elastic quartz capillaries with an inner diameter of 100 μm and an outer diameter of 365 μm, each with a length of 8 cm, place one end of the capillary in a centrifuge tube containing a 110 μm porous silica gel ball, and press a single porous silica gel ball into one end of the capillary, Then use a quartz capillary with an outer diameter of 90 mm to push the single-particle stopper into the end of the capillary as an outlet plunger, and the preparation method of the plunger for ...

Embodiment 2

[0037] Preparation of Capillary Electrochromatographic Columns

[0038] The filler and filling method of the electrochromatographic column are the same as in Example 1, except that the length of the capillary taken is 16cm, and the filling length is 8cm. A 5mm detection window is burned behind the column for ultraviolet detection, and the prepared column is carried out. Evaluation of electrochromatographic separation modes. Sample test results: the sample is a mixture of thiourea, toluene, ethylbenzene, propylbenzene, butylbenzene, and pentabenzene, the buffer system is Tris-HCl (50mM, pH 8.0) / ACN (40 / 60), the separation voltage is 10kV, and the detection wavelength is 214nm. The result is as figure 2 As shown, the column efficiency of the last component, pentylene, is 125,800 plates per meter.

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Abstract

The invention relates to capillary tube chromatographic columns, particularly to a preparing method of high-flux parallel capillary tube chromatographic columns, which is quick and convenient. The to-be-filled particulate filler is added into acetone to be prepared into homogenate; a porous silicon sphere with the particle size greater than the inner diameter of the capillary tube is pressed into one end of the capillary tube, and a single-particle silicon sphere is pushed into the capillary tube to serve as an outlet plunger piston; the inlet end of the capillary tube is communicated with a reservoir, the homogenate is added into the reservoir and placed on a centrifuge to be centrifuged, and a stationary phase enters a capillary tube column as driven by gravity and centrifugal force; the other single-particle silicon sphere is pressed into the inlet end of the filled capillary tube column to serve as an inlet plunger piston; and the prepared capillary tube column is stored for further use.

Description

technical field [0001] The invention relates to a capillary chromatographic column, in particular to a method for rapidly and batchly preparing a capillary chromatographic column. Background technique [0002] Chromatographic column is one of the core components of high performance liquid chromatography and the core of chromatographic separation. Capillary column is a kind of liquid chromatography column. It is usually prepared by elastic quartz tube with an inner diameter of 50-300 μm. Its small column volume can significantly reduce the consumption of column packing and mobile phase, and is especially suitable for the separation of micro and trace samples. It is widely used in liquid chromatography-mass spectrometry and capillary electrochromatography. [0003] Good column preparation technology is the basic factor to obtain high column efficiency. However, due to the small diameter of the column and the need for a special plunger manufacturing process, it is difficult to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/56
Inventor 张博吴清实戴思敏
Owner XIAMEN UNIV
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