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Recycling preparative HPLC (high performance liquid chromatograph) provided with multi-ported valve

A technology of high performance liquid chromatography and cycle preparation, which is applied in the field of cycle preparation high performance liquid chromatography with a multi-port valve, which can solve the problems of complexity and eluent not being recycled, achieve large injection volume and improve separation effect , high separation efficiency

Inactive Publication Date: 2015-05-13
柳仁民
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the eluent is not recycled, and a large amount of eluent is required
In addition, the first elution pump, the second elution pump, and the sampling pump need to be used in combination with multiple six-position three-way valves and one-way six-position valves during the operation process. The operation steps are as many as fourteen steps, which is very complicated.

Method used

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  • Recycling preparative HPLC (high performance liquid chromatograph) provided with multi-ported valve
  • Recycling preparative HPLC (high performance liquid chromatograph) provided with multi-ported valve
  • Recycling preparative HPLC (high performance liquid chromatograph) provided with multi-ported valve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1 as figure 1 As shown, a circulation preparation high performance liquid chromatograph with a multi-way valve and a method for preparing separation and purification, the circulation preparation high performance liquid chromatography is composed of a liquid reservoir M, a high pressure pump P, a sampler S, a chromatographic column It consists of C1 and C2, multi-way valve V, detectors D1 and D2, three-way switching valves T1 and T2, and liquid pipelines.

[0033] The eluent in the reservoir M is transported through the high-pressure pump P through the sampler S, and the sample in the carrier belt sampler S enters the chromatographic column C1 through the multi-port valve V for separation, and the effluent of the chromatographic column C1 passes through the multi-port The valve V enters the detector D1 for detection, and the components in the outflow curve that have reached the purity requirements are cut and extracted through the three-way switching valve T1, an...

Embodiment 2

[0038] Example 2 According to the instrument design, connection and operation mode described in Embodiment 1, reverse-phase chromatographic separation is carried out:

[0039] Reversed-phase chromatography is suitable for separating non-polar or medium-polar compounds, etc. For non-polar or medium-polar compound components with similar properties that are difficult to separate, a double-column circulation preparation high-performance liquid chromatography of the present invention can be used instrument for effective separation. According to the above connection and operation method, chromatographic columns C1 and C2 use stainless steel columns with a diameter of 25mm and a length of 200mm, and the columns are filled with 10mm reverse-phase C18 silica gel packing, and the methanol-water mixed solvent with a volume ratio of 80:20 is used as the eluent. image 3 In the separation process, the detector 1 records the output signal and the schematic diagram of component cutting. The...

Embodiment 3

[0040] Example 3 According to the instrument design, connection and operation method described in Embodiment 1, the chromatographic column and chromatographic conditions in Example 2 are used for separation, no cutting is performed during the separation process, and the corresponding peaks are collected after the separation is complete, and the cycle is repeated 4 times It can effectively separate daidzein and genistein with similar structures. Figure 4 Schematic diagram of the output signal recorded by detector 1 during the separation process. Since the eluent is only consumed when the peak components are collected, and the eluent is recycled at other times, the eluent consumed is very small.

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Abstract

The invention discloses a recycling preparative HPLC (high performance liquid chromatograph) provided with a multi-ported valve as well as a method used for preparation, separation and purification. The recycling preparative HPLC provided with the multi-ported valve comprises a liquid accumulator M, a high-pressure pump P, a sampler S, chromatographic columns C1 and C2, the multi-ported valve, detectors D1 and D2, three-way switching valves T1 and T2, liquid pipelines and the like. The recycling preparative HPLC has the outstanding effects as follows: 1, to-be-separated mixed components are circularly separated only in the two chromatographic columns and are not required for circulation through the high-pressure pump, chromatographic peak broadening is light, the separation efficiency is high, and the separation effect is good; 2, a system is provided with two detectors, peak cutting and circular separation can be accurately controlled, and the separation effect is improved; 3, eluent without the separated components is completely recycled, the consumption of eluent is greatly reduced, and the separation cost is very low.

Description

technical field [0001] The invention relates to a high-performance liquid chromatograph for cyclic preparation and a method for separation and purification thereof, belongs to the technical field of instrument and equipment manufacturing, and is a high-performance liquid chromatography separation and purification device. Background technique [0002] A common preparative high-performance liquid chromatograph is composed of a liquid reservoir, a high-pressure pump, a sampler, a chromatographic column, a detector, a recorder, etc. The eluent in the liquid reservoir is transported by a high-pressure pump, and the eluent in the liquid reservoir The liquid is transported through the sample injector through the high-pressure pump, and the sample in the sample injector is carried into the chromatographic column for separation. The separated components flow out of the chromatographic column and enter the detector in turn, and the corresponding components are collected after the colum...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 柳仁民
Owner 柳仁民
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