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Online low-pressure, middle-pressure and high-pressure combined two-dimension preparation liquid chromatographic system

A technology for two-dimensional preparation and preparation of liquid phase, applied in the field of preparative liquid chromatography system, can solve the problems of high production cost, waste of solvent, complicated and time-consuming and laborious operation, etc., and achieve the effects of saving time, simple operation and reducing production cost.

Inactive Publication Date: 2012-11-21
SOOCHOW HIGH TECH CHROMATOGRAPHY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is time-consuming and labor-intensive to operate, and wastes a lot of solvent, and the production cost is high.
So far, no one has combined low, medium and high pressure preparative liquid chromatography systems to build an online two-dimensional preparative liquid chromatography system for large-scale preparation and production

Method used

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  • Online low-pressure, middle-pressure and high-pressure combined two-dimension preparation liquid chromatographic system
  • Online low-pressure, middle-pressure and high-pressure combined two-dimension preparation liquid chromatographic system
  • Online low-pressure, middle-pressure and high-pressure combined two-dimension preparation liquid chromatographic system

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Experimental program
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Effect test

Embodiment 1

[0023] as attached figure 1 As shown, a two-dimensional preparative liquid chromatography system with online low, medium and high pressure is composed of two low-pressure separation systems and a six-way valve connecting the two separation systems. The No. 1 position of the six-way valve is connected to the No. The outlet of the one-dimensional chromatographic column (column 1) is connected to the detector UV1, the No. 4 position is connected to the inlet of the second-dimensional chromatographic column (column 3), and the No. 5 position is connected to the second-dimensional infusion pump (Pump C, Pump D) , No. 2 and No. 3 positions are connected through external pipelines, and No. 6 position is connected with an external waste liquid collection device.

[0024] In the initial state, six-way valves 1 and 6, 2 and 3, and 4 and 5 are connected, the sample enters the first-dimensional chromatographic column (column 1), and pump A (Pump A) and pump B (Pump B) transport the first-...

Embodiment 2

[0026] Please see attached Figure 2-5 , sample: Florfenicol, the target substance is one of the low-level impurities, and the original HPLC analysis chromatogram is as follows figure 2 shown.

[0027] System composition: an online low and high pressure mixed two-dimensional preparative liquid chromatography system, column 1 is a 30mm×300mm glass chromatographic column filled with 50μm C18 filler; column 2 is a 5mm×50mm stainless steel chromatographic column with a 30μm filler C18 chromatographic stationary phase; column 3 is a 10mm×250mm stainless steel chromatographic column filled with 5μm C18 filler. Both UV1 and UV2 are dual-wavelength ultraviolet detectors.

[0028] Chromatographic conditions: the detection wavelength is 225nm, 230nm. Both the first and second dimension chromatographic systems use water and methanol as mobile phases, and gradient elution.

[0029] Refer to attached Figure 4 , which is the second-dimensional chromatogram obtained by using the syste...

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Abstract

The invention relates to an online low-pressure, middle-pressure and high-pressure combined two-dimension preparation liquid chromatographic system. Two one-dimension low-pressure, middle-pressure and high-pressure preparation liquid chromatographic systems are organically combined through a six-way valve and software. Pressure used by a second dimension system is not lower than pressure used by a first dimension separation system. When the first dimension system and the second dimension system are low-pressure or middle-pressure preparation liquid chromatographic systems, through switching the six-way valve, target compound directly enters a second dimension chromatographic column for second dimension separation after first dimension separation; and when pressure used by a second dimension separation system is higher than pressure used by the first dimension separation system, a trapping column is connected on the six-way valve, the target compound is adsorbed on the head of the trapping column after the first dimension separation, and then the target compound enters the second dimension chromatographic column for second dimension separation. The invention has the advantages thatthe contradiction between sample injection volume and separation capacity is solved, the large sample injection volume is ensured and the separation capacity of the preparation chromatographic systemis greatly improved; the system structure is simple and the establishment is easy; the operation is simple and convenient and the automation can be easily realized; and the application scope is wide.

Description

【Technical field】 [0001] The invention relates to the field of preparative liquid chromatographic systems, in particular to a two-dimensional preparative liquid chromatographic system combining on-line low, medium and high pressure. 【Background technique】 [0002] Preparative liquid chromatography is a separation technique for the purpose of obtaining pure samples. Since it was applied to the separation of pigments in the 1930s, it has made great progress. In the 1980s, high-performance preparative liquid chromatography developed rapidly in the pharmaceutical industry, and in the 1990s, it was widely used in the separation and purification of proteins. Today, preparative chromatography is used in almost every field of social production and life, such as the separation and purification of secondary metabolites, natural products, macromolecular compounds, and some important pharmaceutically active proteins, biotherapeutics, and diagnostic reagents. However, compared with anal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/08
Inventor 邵平戈兆松王安王芸张维冰
Owner SOOCHOW HIGH TECH CHROMATOGRAPHY
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