A double-column circulating preparative high-performance liquid chromatograph and a method for preparative separation and purification

A high-performance liquid chromatography and cyclic preparation technology, applied in the field of high-performance liquid chromatography separation and purification devices, can solve the problems of complexity and no recycling of the eluent, and achieve a large injection volume, improved separation effect, and high separation efficiency. Effect

Inactive Publication Date: 2016-04-13
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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  • A double-column circulating preparative high-performance liquid chromatograph and a method for preparative separation and purification
  • A double-column circulating preparative high-performance liquid chromatograph and a method for preparative separation and purification
  • A double-column circulating preparative high-performance liquid chromatograph and a method for preparative separation and purification

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Experimental program
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Effect test

Embodiment 1

[0033] like figure 1 As shown, a double-column circulation preparation high-performance liquid chromatograph and a method for preparing separation and purification, the double-column circulation preparation high-performance liquid chromatography is composed of a liquid reservoir M, a high-pressure pump P, a sampler S, and a chromatographic column C1 and C2, flow switching valves F1-F8, detectors D1 and D2, collection switching valves S1 and S2, three-way switching valve T, liquid pipelines, etc.

[0034] The eluent in the reservoir M is transported through the high-pressure pump P through the sample injector S, and the sample in the carrier tape injector S enters the chromatographic column C1 through the valve F1 for separation, and the effluent of the chromatographic column C1 is detected by the detector D1 , the components that have reached the purity requirements in the outflow curve are cut and extracted through the collection switching valves S1 and S2, and the overlappin...

Embodiment 2

[0039] According to the instrument design, connection, chromatographic column and chromatographic conditions described in Embodiment 1, without cutting and separating the enantiomers of rosiglitazone, image 3 Schematic diagram of the output signal recorded by detector 1 during the separation process. The complete separation of the enantiomers of rosiglitazone can be achieved by 4 cycles, the sample is not cut during the separation process, and the peak components are collected after the final separation is complete. Since the eluent is only consumed when the peak components are collected after the final separation is completed, and the eluent is recycled at other times, the eluent consumed is very little.

Embodiment 3

[0041] According to the instrument design, connection and operation mode described in Embodiment 1, reverse-phase chromatographic separation is carried out:

[0042] 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. Figure 4 In the separation process, the detector 1 records the output signal and the schematic diagram of component cutting. The front pe...

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Abstract

The invention discloses a double-column cyclic preparation HPLC (high performance liquid chromatograph) and a method for preparation, separation and purification. The double-column cyclic preparation HPLC comprises a liquid storage device M, a high-pressure pump P, a sample injector S, chromatographic columns C1 and C2, flow path switching valves F1-F8, detectors D1 and D2, collecting switching valves S1 and S2, a three-way switching valve T, a liquid path pipeline and the like. The HPLC has the outstanding effects as follows: 1, a to-be-separated mixed component is only subjected to cyclic separation in the two chromatographic columns and is not required to be circulated by the high-pressure pump, the chromatographic peak broadening is light, the separation efficiency is high, and the separation effect is good; 2, a system can cut and draw out a component meeting the purity requirement by the aid of the collecting switching valves, the peak broadening overlapping phenomenon is eliminated, the sample size is large, the separation efficiency is high, and the cost is low.

Description

technical field [0001] The invention relates to a double-column circulation preparation high-performance liquid chromatograph and a method for preparation, separation and purification, which belong to the technical field of instrument and equipment manufacturing, and are 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...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/10B01D15/24
Inventor 柳仁民
Owner 柳仁民
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