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Vacuum auxiliary-solvent evaporation interface combined with two-dimensional liquid chromatography

A vacuum-assisted liquid chromatography technology, applied in the field of two-dimensional liquid chromatography, can solve problems affecting the second-dimensional separation efficiency, peak shape distortion, and band broadening

Inactive Publication Date: 2009-09-30
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when the two dimensions use chromatographic columns with similar inner diameters, the sample volume cut into the second dimension is far greater than the maximum allowable injection volume of the second dimension column; at the same time, a large number of immiscible mobile phases or mobile phases with greatly different viscosities enter When the second-dimensional chromatographic column is used, the separation performance of the second dimension will be affected (column efficiency is severely reduced), and peak shape distortion, band broadening and large-scale fluctuations in the baseline will occur on the detector.
[0006] 3) The second-dimensional analysis speed limits the separation speed of the two-dimensional combined overall
However, the method of post-column dilution in the first dimension also has disadvantages: when the first dimension uses gradient elution, the reproducibility of the two-dimensional separation is poor

Method used

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  • Vacuum auxiliary-solvent evaporation interface combined with two-dimensional liquid chromatography
  • Vacuum auxiliary-solvent evaporation interface combined with two-dimensional liquid chromatography
  • Vacuum auxiliary-solvent evaporation interface combined with two-dimensional liquid chromatography

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Experimental program
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Embodiment 1

[0027] Experimental device such as figure 2 Shown, with high-pressure liquid chromatography pump as the first dimension infusion pump, the first six-way valve 1 is as the first dimension liquid chromatography sampling valve, and the first dimension chromatographic column uses the cyano group stationary phase column, and column size is ( 250 mm x 4.6 mm i.d., 5 μm) with an ultraviolet-visible absorptiometry (UV-Vis) detector as the detector for the first dimension chromatography. Use another six-way valve 100 as an interface valve, and the evaporation quantitative tube connected to it is a 120mm×1.0mm i.d. stainless steel tube. A constant temperature water bath is used to realize the constant temperature of the evaporation quantitative tube. 1Pa, pumping speed 2L / s) to evacuate the evaporation quantitative tube. A high performance liquid chromatograph with UV-Vis detector is used as the second dimension liquid chromatographic system. A ten-way valve (III) is used as a switch...

Embodiment 2

[0029] The experimental device and method are the same as in Example 1, and the ultrasonic extract of angelica n-hexane (90% n-hexane / 5% dichloromethane / 5% isopropanol) is analyzed. The first dimension normal phase chromatogram is shown in Figure 4 A, the analysis conditions are: chromatographic column, cyano column (150mm×2.0mm i.d., 5μm); mobile phase, 90% n-hexane / 5% dichloromethane / 5% n-propanol; flow rate 0.18mL / min; detection wavelength 254nm; injection volume 20μL. The chromatogram of reverse-phase direct injection is 4B, and the analysis conditions are: mobile phase, A, 5% methanol; B, methanol; gradient elution program, 0-40min, 40%B linearly increased to 100%B; 40-50min, 100% B; 50-55min, linearly decreasing to 40% B; flow rate 0.8mL / min; detection wavelength 254nm; injection volume 20μL. Cut the first-dimensional separation components into 10 parts, and enter the second-dimensional separation after passing through the interface respectively. See the spectrum Fi...

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Abstract

The invention relates to two-dimensional liquid chromatography, in particular to a vacuum auxiliary-solvent evaporation interface combined with the two-dimensional liquid chromatography. As an interface for fraction switching or column switching, the interface is mainly applied to the two-dimensional liquid chromatography, and comprises a six-way valve, a fraction collecting-evaporating quantification pipe, a heater and a vacuum pump. The interface has the advantages of solving the switching of a two-dimensional mobile phase, reducing the volume of secondary-dimensional sample introduction, increasing the concentration of samples and improving detection sensitivity. A two-dimensional liquid chromatography system using the vacuum auxiliary-solvent evaporation interface is suitable for separating and analyzing non-volatile or high-boiling-point compounds.

Description

technical field [0001] The invention relates to two-dimensional liquid chromatography, in particular to a vacuum-assisted solvent evaporation interface. This interface is mainly used for the combination of normal phase liquid chromatography and reversed phase liquid chromatography. It not only realizes the conversion of the two-dimensional mobile phase, but also reduces the injection volume of the second dimension, increases the concentration of the sample, and improves the detection efficiency. sensitivity. The two-dimensional liquid chromatography system using the vacuum-assisted solvent evaporation interface is suitable for the separation and analysis of non-volatile or high boiling point compounds. Background technique [0002] Limited by the pressure resistance of the instrument itself and the size of the chromatographic column, the peak capacity of one-dimensional separation of liquid chromatography cannot be greatly improved. When one-dimensional liquid chromatograp...

Claims

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Application Information

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IPC IPC(8): G01N30/00
Inventor 关亚风徐媛丁坤王华
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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