A general-purpose preparative two-dimensional liquid chromatography device and its operating method

A technology of two-dimensional liquid chromatography and operation method, which is applied in the field of purification and purification of analytical chemical standard products, and achieves the effects of convenient operation, wide application range and compact structure

Active Publication Date: 2017-10-20
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparative two-dimensional liquid chromatography device with a high degree of automation has not been reported at home and abroad.

Method used

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  • A general-purpose preparative two-dimensional liquid chromatography device and its operating method
  • A general-purpose preparative two-dimensional liquid chromatography device and its operating method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] according to figure 1 The shown device structure connects each component to obtain the general preparative liquid chromatography device of the present invention:

[0033] The interface ① of the six-way multi-position valve a is connected to solvent bottle a, the interface ② is connected to solvent bottle b, and the interface ③ is connected to solvent bottle c; the inlet of the constant flow pump is connected to the common outlet in the middle of the six-way multi-position valve a, and the outlet and the flow path are selected The common inlet C21 of the multi-position valve is connected; flow path selection The multi-position valve has 4 different flow paths, flow path 1 is connected to the first-dimensional chromatographic system, and is connected to the manual six-way sampling valve b and the normal phase chromatographic column successively from the inlet end , and then connected to the outlet port, the flow path 3 is connected to the second-dimensional chromatographi...

Embodiment 2

[0040] One-dimensional normal phase separation: target to be purified: 15mg / mL caffeine in dichloromethane solution.

[0041] The six-way multi-position valve a is connected to the normal phase solvent (methanol 10%: dichloromethane 90%), the flow path is connected to the No. 1 flow path of the multi-position valve, and the sample is injected into the normal phase chromatogram through the six-way multi-position valve b The column (20*250mm high-efficiency silica gel column) is used for separation, the flow rate is 12mL / min; the injection volume is 2mL, the waste liquid is discharged through the interface ① of the six-way multi-position valve c, and the target components are collected through the interface ③, the target collection interval: 6.80- 8.25min. The actual separation situation is as follows figure 2 Shown: Trace impurities in caffeine are separated, and a 30mg sample can be purified in one injection. The operation is automatically executed by the self-compiled contr...

Embodiment 3

[0043] One-dimensional reversed-phase separation: target substance to be purified: 5 mg / mL capsaicin in methanol solution.

[0044] The six-way multi-position valve a is connected to 55% acetonitrile, and the flow path selection multi-position valve No. 3 is connected to the flow path. The sample is placed in the automatic sample concentration pool, and the sample passes through the automatic metering pump composed of a low-pressure metering pump and six-way multi-position valve d. The sampling device is separated on the second-dimensional reverse-phase chromatographic column (20*250mm high-efficiency C18 column), the flow rate is 16mL / min; the injection volume is 8mL. The waste liquid is discharged through the interface ⑤ of the six-way multi-position valve c, and the target components are collected through the interface ⑥. The target collection interval: 10.50-14.00min. The operation is automatically executed by the self-programmed control software. In the sample loading sta...

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Abstract

The present invention provides an automatic two-dimensional high-performance liquid phase preparative chromatography device, which can be used for automatic purification of laboratory-scale (<1 g) chemical standards. The device includes a large-flow constant-flow pump, a liquid multi-position valve, a high-efficiency preparative chromatographic column, an ultraviolet detector, and a self-made two-dimensional liquid chromatography interface. After the target substance is separated by the first-dimension chromatography, the solvent is removed in the self-made two-dimensional liquid chromatography interface device (9), and the second-dimension separation is carried out after dissolving with the mobile phase of the second-dimension chromatography. The device can realize automatic solvent selection; automatic flow path and chromatographic column selection; automatic collection of target components. The purified target compound solution will be collected at the designated receiving location, and a high-purity standard can be obtained after simple rotary evaporation. The advantages of this device are: 1. Low cost, compact structure and light weight; 2. Simple to use and high degree of automation; 3. There are three different purification operation modes: one-dimensional normal phase, one-dimensional reverse phase, and two-dimensional separation, with a wide range of applications , the solvent cost is low, and the purification effect is good.

Description

technical field [0001] The invention belongs to the field of refining and purifying analytical chemical standard products, and mainly relates to the purification and refining process of laboratory-scale (<1g) high-purity analytical chemical standard products, which can refine low-purity raw materials into high-purity analytical standard products. Specifically, the present invention is a general-purpose preparative two-dimensional liquid chromatography device and its operating method and application. Background technique [0002] High-purity standards are an important material guarantee for various qualitative and quantitative analyses. High-efficiency preparative chromatography is currently a widely used purification technique. Compared with conventional purification methods such as recrystallization, high-efficiency preparative chromatography has the advantages of good resolution and fast speed. In order to further improve the separation efficiency of liquid chromatogr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/14B01D15/24G01N30/06
Inventor 王龙星袁和平里东张海军陈吉平
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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